(32hI) Jones, K., Chem Brit., 5, 552 (1969):
(33x1) hawahara, F. K., Envzron. SCZ. T~chnol, 3, 150 (1969). (34M) Kotnick, G., Scheck, H. F., Instrum. Techno/., 16 (9), 52 (1969). (35hI) Krichmar, S . I., Stepanenko, K. E., Khzm. Prom, 1969,235. (36M) Langermeersch, van, A., Chim. Anal. (Parts), 50, 3 (1968). (37hI) Lauer, G., Osteryoung, R. A., ANAL.CHCM., 40, 30A (1968). (38h2) Lawerenz, A., Fortschr. Wasserchem. Ihrer Grenzgeb., 1968, 21. (3931) Levine, I. S., Sutton, W. G., Oil Gas J., 67 (13), 63 (1969). (40M) Lysyj, I., Nelson, K. H., Newton, P. R., J . Water Pollut. Contr. Fed., 40, It181 (1968). (4111) hlaehler, C. Z., Greenberg, A. E., J . Santt. Eng. Dzv., (Amer. SOC.Civil Eng.), 94,969 (1968). (42M) XIcKinney, R . W., Garst, G. It., Raver, R. E., Harris, W. O., J . Gas Chromatogr., 6, 115 (1968). (43hI) MacPhee, R . D., Kuramoto, &I., J . Air Poll ut. Contr. Ass., 19,443 (1969).
(44M) Marletta, G. P., Gabrielli, L. F., Tec. Jtal., 34,307 (1969). (45M) Marten. J. F.. Ind. Chim. Belae. 32.. 1319 (1967). (46M) Matthews, P. J., J. A p p l . Chem. (London), 20, 87 (1970). (47M) Mattson, J. S., Mark, H. B., Jr., Kolpack, R. L., Schutt, C. E., ANAL. CHEM.,42, 234 (1970). (48M) Otcasek, It. A., S A E (SOC.Auto. Eng.) Spec. Publ., 350, (1969). (49M) Ramsdale, S. J., Wilkinson, R. E., J. Inst. Petrol., 54, 315 (1968). (50M) Raymond, A. J., Lawrey, I). M. G., Mayer, T. J., J . Chromutogr. Sci., 8 , l(1970). (5lM) Saltzman, R. S., Anal. Instrumen., 6,79 (1968). (52hI) Scaringelli, F. P., Rehme, K. A,, ANAL.CHEM.,41,707 (1969). (.53M) Schneider, W., Chem. Tech. (Berlin),20, 299 (1968). (54M) Sher, J. A., Oil Gas J . , 66 (36), 93 119681. (55hI) Sono, K., Iwashige, H., Kyushin, S., Kogyo Kagaku Zasshi, 72, 801 (1969). I
,
\ - - - - , -
(56M) SOOS, K., Cieleszky, V., K o ~ . Ert., 11, 100 (1969). (57M) Steger, E., Kahl, H., Chem. Tech. (Berlin),21, 483 (1969). (58M) Sugar, J. W., Conwa , R. A,, J . Water Pollut. Contr. F e z 40, 1622 (19681. \---_,
(.59M) Taras, M. J., Blum, K. A,, ibid., p R405. (60M) Templeman, G. C., ASTM (Amer. Soc. Test. Mater.) Comm. D-2 Symp., New Orleans, 1968, Preprint, 32 pp. (6lM) Tunnicliff, D. D., Wadsworth, P. A., ANAL.CHEM.,40, 1826 (1968). (62M) Vasil’eva, V. V., Nikolaeva, N. G., Ivanova, T. S., Nejtepererab. Neftekhim. (Moscow), 1969, 52; A.P.I.A., 16, 14438 (1969). (63M) Weihman, K. F., Davis, E. N., Wertzler, R., Nat. Petrol. Refiners Ass. Computer Conf., Phila., 1968, Pap. CC68-94,21 pp. (64M) Wernimont, G., ASTM (Amer. SOC.Test. Mater.) Comm. D-2 Symp., New Orleans, 1968, Preprint, 64 pp. (65M) Yoshii, T., Katsuda, K., Ueda, K., Kogyo Yosui, 1967, 72.
Pharmaceuticals and Related Drugs 1. W. Sutherland,
D. E.
Williamson, and I. G. Theivagt,
Analytical Research Department, Abbott laboratories, North Chicago, 111.
T
HIS SURVEY INCLUDES analytical methods and related topics of pharmaceutical interest t h a t have appeared since the last published review (1500), or were not included in the previous reviews, and covers t h e literature to June 1970. The same tabular format is retained from the last review. References to the analysis of pharmaceuticals in biological media are denoted b y a superscript B. Such references are restricted to t h e determination of administered drugs and metabolites. Numerous reviews of interest to analytical chemists working in the drug field have appeared. Automated techniques in pharmaceutical analysis were presented, including both continuous flow and discontinuous analysis (1136). I n the fundamental analytical reviews on chromatography (2549), ion exchange (1150), and electrophoresis (1985), applications of t h e respective techniques to pharmaceuticals were discussed. Pertsev (1568) has presented a general review of thin-layer chromatography and its use in pharmaceutical analysis. M a n y references to drugs are found in Haywood’s (805) and Stahl’s (1948) books on thin-layer chromatography. Several applications of chromatography to drugs are described in books by Smith (1924) and blarinetti (1258). Still presented in the Journal of Chromatography are the bibliography and chromatographic sec-
206 R
0
tions which frequently list current applications of t h e various chromatographic techniques to pharmaceuticals. Comprehensive reviews have appeared on gas chromatography in pharmaceutical analysis (1127, 1329). Kroman and Bender, in their book “Theory and Application of Gas Chromatography in Industry and Medicine,” discuss applications in drug research, toxicology, drug metabolism, and new drugs (1113). The increasing use of derivatization for previously nonchromatographable compounds is exemplified by Sennello’s application to vitamins (1839). Reviews on nonaqueous titrimetry applied to drug analysis have appeared (651, lS43). The applications of spectrophotometric titrations (1884) and high-frequency titrations (1711) to pharmaceuticals have also been reviewed. Recent developments in t h e field of ultraviolet spectrometry have been reviewed, including applications to pharmaceutical analysis (404). Photometry in t h e analysis of drugs was reviewed b y Yaskina and Lirova (2311). I n Bouche’s review of infrared spectrophotometry in drug analysis (248), he discussed the place of infrared spectrophotometry in pharmacopeias and other official texts on pharmaceuticals. T h e fluorometric analysis of vitamins, steroids, hormones, and other pharmaceuticals was reported in the review by White
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
and Weissler (8258). An introduction to fluorometry with applications for determining pharmaceuticals was described by Xirau-Vayreda (2278). T h e spectroscopy of amines of pharmaceutical interest was reviewed by Eisdorfer, Warren, and Zarembo (509). Both t h e qualitative and quantitative aspects of the various techniques, UV, I R , N M R , Raman and mass, were described. The applications of modern electroanalytical techniques to pharmaceutical chemistry was covered by Adams ( 5 ) . Discussed were the fundamentals of voltametry, comparison of potentiometry and voltammetry, response characteristics of electrodes, and potentialities and shortcomings of electroanalytical techniques. General articles, discussing the present status and progress of pharmaceutical analysis, are presented in a number of papers (548, 1006, 1007, 1589, 1590, 1591, 1593, 1595, 1840, 2106). Schmitt and Mathis have provided a survey on t h e analytical methods for antibiotics reported during the last ten years (1815). The identification of drugs has received attention with the recent publications by Clarke (367),Fulton (618),and Sunshine (8002). Even though written for the toxicologist, all three books have a wealth of information useful to those concerned with drug identification and analysis in general.
Gearien and Grabowski (640) have published the book “Methods of Drug Analysis.” T h e book “Pharmaceutical Chemistry: Instrumental Techniques,” by Chatton (337), has ahso been published. New editions of two general handbooks are now available: t h e eighth edition of “The M.erck Index of
Chemicals and Drugs” (1964), and t h e fourteenth edition of “Remington’s Pharmaceutical Sciences” (834). Discussions of the analytical methods and contents for t h e second edition of the International Pharmacopeia (70), and for t h e seventh edition of t h e German Pharmacopeia (816) have been
Table 1. Compound or Class Alkaloidal amines Bisnorephedrine Colchiceine Colchicine Democolcine Ephedra alkaloids Ephedrine
Methylephedrine Norephedrine Norpseudoephedrine Pseudoephedrine Alkaloids, general methods
Alkaloids miscellaneous Aconitum alkaloids
presented. T h e United States Pharmacopeia, Volume XVIII (2148) and The National Formulary, Volume XI11 (1404) have appeared. T h e number of monographs in t h e new National Formulary have increased considerably, reflecting a broader admission policy. (Text cmtinued on page 241 R )
Alkaloids
Method or Subject
Reference
Chromatographic, thin layer; fluorometric S ectrophotometric, ultraviolet Cfuomatographic gel; ion exchange Colorimetric Spectrophotometric, ultraviolet Spectrophotometric, ultraviolet Chromatographic, thin layer Chromatographic, gas Chromatographic, ion exchange Chromatographic, paper Chromatographic, thin layer
(1706)
Colorimetric Distillation, steam Distribution coefficients Electrophoretic, paper; of W-labelled Extractive Fluorometric Identity Neutron activation analysis; of silver complex Resolution of racemic mixtures Spectrophotometric, infrared Spectrophotometric, ultraviolet Volumetric, acid-base Volumetric, acid-base, nonaqueous Volumetric, conductometric Colorimetric Chromatographic, thin layer; fluorometric Neutron activation; of silver complex Chromatographic, thin layer Electrophoretic,. paper Chromatographic, column Chromatographic, gas Chromatographic, gel Chromatographic, paper Chromatographic, thin layer
Colorimetric Complexometric Detection Electrophoretic, paper Extractive Fluorometric Identification Microcrystallographic Polarographic Reaction, with iodine Reineckates Review Review, critical Spectrophotometric, infrared Tetraphenylborate reagent, use of Volumetric, acid-base, nonaqueous Volumetric, conductometric Volumetric, coulometric Volumetric, oscillometric Volumetric, ultramicro
Chromatographic, gas Chromatographic, paper Acronine Chromatographic, gas Amaryllidaceae alkaloids Chromatographic, gas Distribution coefficients Anabis aphylla alkaloids Chromatographic, thin layer Distribution coefficients Boldine Chromatographic, paper Analysis of pharmaceuticals in biological media.
(613, 1398, 2266) (563,64TB,137SB) (137SB,1638) ( g w , 1.984, 1339, 1373, 1496, 1706, 1782. 2806. 8886)
(1860, 1421) (1063)
(1706) (836)
%:I
( i h ij
(264, 8 9 ~ 589gB, ~ , 1166) (647~) (198, 737, 1412, 1418, 1637, 1988) (836, 430, 626, 610, 646, 737, 797, 848, 937. 978. 1166. 1168. 1260. 1327. 1339, 1412, 1488, 161dB, 1671, 1?3l1733, 1826, 2256, 2862, 2880) (198, 1844) (2318) (1418, 1676) (9076. 2077B. 2202) (496,497, 1,&8, 161dB, 1844) (1161)
(57,406, 646, 1004, 1744) (646) (1101, 2883) (2262) (406) (37,1671,1676) (294) (998) (1138) (637, 1743)
(60% (1626) (602) (1841) (2021) (1001) (616) (1183,8018) (1677) (694) (1677) (1730)
(Continued on next p a g e )
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
207 R
Compound or Class Capsicum Cascara Catharanthus roseus alkaloids Cauloph llum thalictroides Condelp&ne Conium alkaloids AY,K’-Diallylbis-nortoxiferine Erythrophleum alkaloids Euphylline Folia alkaloids Glaucine Glucoside alkaloids Harman Harmine Ligularia clivorium Mescaline Nitragyna oxindole alkaloids
Noscapine Pachy carpine Pericallane Peyote alkaloids Phenolic alkaloids Pilocarpine
Rhamnus bark alkaloids Securinine
Serratinine Sparteine Spherophysine Spherophysine benzoate Tazettine Thujyl compounds Valerianceae drugs Wrightia tinctoria Indole alkaloids Ajmalicine Ajmaline
Brucine
Ergot alkaloids
Table I. Alkaloids (Continued) Method or Subject Chromatographic, gas Review Colorimetric; extractive Chromatographic ; spectrophotometric Chromatographic, column Colorimetric Chromatographic, gas; radiometric Chromatographic, thin layer Review Volumetric, acid-base, complexometric Chromatographic; thermal analysis Chromatographic, thin layer Review Chromatographic, thin layer Colorimetric Chromatographic, thin layer Dialvsis Flu&ometric Chromatographic, thin layer Colorimetric Densitometric Spectrophotometric, ultraviolet Spectrophotometric, infrared Distribution coefficients Volumetric, acid-base, nonaqueous Identification; physical properties Chromatographic, gas Chromatographic, gas Chromatographic, thin layer Automated analysis Chromatographic, paper Chromatographic, thin layer Microcrystallographic Nuclear magnetic resonance Spectrophotometric, infrared Spectrophotometric, volumetric Volumetric, acid-base, nonaqueous Chromatographic, thin layer; review Colorimetric Chromatographic, paper Chromatographic, thin layer Colorimetric Extractive Mass spectrometric Chromatographic, partition Colorimetric, ion-pair Volumetric, ox.-red. Volumetric, acid-base, nonaqueous Chromatographic, gas Chromatographjc, thin layer Chromatographic; spectrophotometric Chromatographic, thin layer Chromatographic, thin layer Spectrophotometric, ultraviolet Chromatographic, paper Chromatographic, thin layer Colorimetric Colorimetric, semi-quantitative Extractive, ion-pair Spectrophotometric, infrared Spectrophotometric, ultraviolet Chromatographic, paper Chromatographjc, partition Chromatographic, thin layer Review Spectrophotometric, infrared SDectroDhotometric. ultraviolet StabilitG Volumetric, complexometric Volumetric, thermometric Chromatographic Chromatographic, gel Chromatographic, paper Chromatographic, thin layer
Colorimetric Identification; general tests Stability kinetics Lysergic acid diethylamide Chromatographic, gas Chromatographic, gel Chromatographic, Ion exchange Analysis of pharmaceuticals in biological media.
Reference (829) (1206) (1767) (1276) (686)
(1576) (1269) (766 ) (I366 ) (1026) (1947) (1966)
(1601,1860,1862,1865,1866,1867) (661 ) (1861. 1866) (1860; 1864) (2066) (1677) (637) (649)
(1202, 1866) (1202) (389) (236, 389, 1202) (389)
g$:{ $2 1202) (1930, 1968,
8133)
(1989) (761) (329) (1782) (476, 8208) (1962)
):!it?) (11)
(66) (986 1 (10, 660, 764, 836, 836, 936, 1787, 2969, 2303) (10, 11, 836, 836, 2337) (1699) {::b6, 1166) )%?B)
(Continued on next page)
208R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
Compound or Class
Nuxvomica alkaloids
Phalaris arundinacea alkaloids Physostigmine
Rauwolfia alkaloids
Reserpine
Strychnine
Vinca minor alkaloids
Yohimbine alkaloids Isoquinoline alkaloids Apomorphine
Table I. Alkaloids (Continued) Method or Subject Chromatographic, paper Chromatographic, thin layer Collaborative study; identification Fluorometric Mass spectrometric Review Spectrophotometric, infrared Spectrophotometric, ultraviolet Chromatographic, column Chromatographic, gas Chromatographic, paper Colorimetric, ion-pair Extractive Identification ; separation of minor alkaloids Stability Chromatographic, gas Chromatographic, gas Chromatographic, paper Chromatographic, thin layer Colorimetric Fluorometric Microcrystallographic Chromatographic, paper Chromatographic, thin layer Colorimetric Electrophoretic Mass spectrometric Microscopic, quantitative Nuclear magnetic resonance Polarimetric; spectrophotometric Review Spectrophotometric, ultraviolet Automatic analysis Chromatographic, column Chromatographic, partition column Chromatographic, paper Chromatographic, thin layer Collaborative study Colorimetric Electrophoretic, paper Fluorometric Identification Spectrophotometric S ectrophotometric, ultraviolet &lumetric, ox.-red. Chromatographic, gas Chromatographic, paper Chromatographic, thin layer Colorimetric, ion-pair Identification Micro crystallographic Microdetermination, volumetric Review Spectrophotometric, infrared Spectrophotometric, ultraviolet Stability Volumetric, acid-base Chromatographic, paper; colorimetric Extractive, countercurrent Mass spectrometric Optical rotatory dispersion Stereochemical Chromatographic, gas Chromatographic, paper
Chromatographfc, paper Chromatographic, thin layer Colorimetric Spectrophotometric, ultraviolet Berberine Chromatographic, paper Chromatographic, thin layer Colorimetric Electrophoretic, paper Fluorometric Review Berberis vulgaris alkaloids Electrophoretic, paper Canadine Review Chelidonium majus L. alkaloids Chromatographic, thin layer Codeine Chromatographic, column Chromatographic, gas Chromatographjc, gel Chromatographic, paper Analysis of pharmaceuticals in biological media.
Reference (1198,1373) (1166,1373) (1198) (6611 (1.619) (ii66,’ 1198) (1166,1310 ) (1198) (1344) (1911 (1962,2208) (1179) (496) (1344) (1962)
(389,’ 786,1606, 1671) (389,768,1127) (1196B, 1198)
(119,769,1131) (389)
(936) 11697) (1627,’ 1963) (389,1111) (769) (191) (1418,1919,1930,1968,2133,2208) (284,761,1146) (19.4,1179) (1004)
(1146) (1660) (368)
(1781) ii426j (1962) (1660,1981) (2342,2343) (933) (1076) (2114) (1076) (141) (1930) (1418) (636) (1696) (1077) (1930) (647,962,1313) (9661 (966) (1313) (647) (9661 (647) (477) (938,1647,6163,6306) (436,1614=,2266) (666,668) (1886,1008) (Continued on next page)
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
209R
Table 1. Compound or Class
Corydaline Cryptopine Diacetylmorphine (heroin) Diamorphine
Dicen trine Dihydrocodeine Dihydrocodeinone Dihy droxycodeinone Dilandid Ethylmorphine
Galan thamine Galan thine Hydrastine
Hydrastinine Laudanosine Lemoran Levorphanol Lycoramine Lycorine Lycoris radiata Morphine
Alkaloids (Continued)
Method or Subject Chromatographic, thin layer Chromatographic, ion exchange Colorimetric Colorimetric, ion-pair Densitometric Dihydrocodeinone, in Distribution coefficients, ion exchange Extractive Fluorometric Gravimetric Identification Spectrophotometric, infrared Spectrophotometric, ultraviolet Volumetric, acid-base Volumetric, acid-base, nonaqueous Volumetric, conductometric; oscillometric Volumetric, ion-pair Chromatographic, paper Chromatographic, paper Chromatographic, thin layer Chromatographic, column Chromatographic, gas Chromatographic, thin layer Spectrophotometric, infrared Spectrophotometric, ultraviolet Stability Chromatographic, paper Identification; derivatiaation Morphine contamination of Spectrophotometric infrared Spectrophotometric: infrared Colorimetric Chromatographic, thin layer Chromatographic, thin layer Colorimetric Extractive, ion-pair Morphine contamination of S ectrophotometric, ultraviolet &urnetric, acid-base, nonaqueous Chromatographic, gas Extractive Chromatographic; spectrophotometric Chromatographic, paper Chromatographic, thin layer Fluorometric Review Spectrophotometric, ultraviolet Chromatographic, paper; fluorometric Chromatographic, thin layer Colorimetric Chromatographic, thin layer Chromatographic, thin layer Chromatographic, thin layer; colorimetric Chromatographic, gas Chromatographic; spectrophotometric Chromatographic, thin layer; colorimetric Chromatographic, gas Chromatographic Chromatographic, column Chromatographic, gas Chromatographic, gel Chromatographic, ion exchange Chromatographic, paper Chromatographic, preparative Chromatographic, thin layer Colorimetric Densitometric Ethylene oxide, effect on Extractive Fluorometric Gravimetric Identification Nuclear magnetic resonance Polarographic Spectrophotometric, infrared Spectrophotometric, ultraviolet
Morphine derivatives
Chromatographic, column Chromatographic, thin layer * Analysis of pharmaceuticals in biological media.
210 R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
Reference (96, 884, &OB, 508, 656, 788, 768, 938, 1339, 1614, 1681, 1782, 1811, 1950, 2063, 2206, 8207, 2886) (363. 6L7B) (190; 768, 844, 1618, 2286) (1969) (608, 1886) (1387) (668)
(113. 190) (6077 ‘ (i13j (338) (1387, 1788) (607, 640, 666)
i74j (71) (1387) ( 1385) 8286)
(2019) (1383) 121171
(962 ’ (2oOiiq (1819) (1e98, 19.m~816s)
[@;: ;:if)
(1464B) (14MB,8008) (8306) (@OB,636, 814, 146~5~, 151dB, 1621, 1886, 1950, 8063, 8089, 2807, 2236) (437, 1460B, 8146) (1071, 1886) (1777)
yg
%;)
(1697. 8163) (74, 607) ’ (1666) (14% 8344) (998) (488, 607, 1077, 1654, 1983, 2023, 2836, 287.e) (938) (246, 428, 635, 963, 1464B, 146bB)
(Continued on next page)
Compound or Class Nalorphine Narceine Narcotine (noscapine)
Narcotoline Opium
Opium alkaloids
Papaverine
Table 1. Alkaloids (Continued) Method or Subject Colorimetric S ectrophotometric, ultraviolet Cfwomstogrsphic, thin layer Colorimetric Chromatographic, paper Chromatographic, thin layer Colorimetric; extractive Chromatographic, gel Chromatographic, paper Chromatographic, thin layer Colorimetric Distribution coefficients, ion exchange gels Electrophoresis, paper Fluorometric Spectrophotometric, infrared ~: Spectrophotometric, ultraviolet Chromatographic, paper Chromatographic, column Chromatogra hic, thin layer Ethylene oxiie, effect on Extractive Porphyroxine in; chromatographic, thin layer SDectroDhotometric. ultraviolet C'hromatographic, gas Chromatographic thin layer Distribution coedcients, ion exchange gels Extractive Autooxidation Chromatographic, gel Chromatographic, ion exchange Chromatographic, ion exchange paper Chromatographic, paper Chromatographic, thin layer Colorimetric Colorimetric, ion-pair Densitometric Distribution coefficients, ion exchange gels Electrophoretic, paper Fluorometric Microcrystallographic Polarographic Spectrophotometric, infrared Spectrophotometric, ultraviolet S ot tests olumetric, acid-base Volumetric, acid-base, nonaqueous Volumetric, complexometric Volumetric, coulometric Volumetric, ox.-red. Chromatographic, paper Chromatographic, thin layer Electrophoretic, paper Polarogra.phic Volumetric, acid-base Volumetric, conductometric, oscillometric Chromatographic, thin layer Chromatographic, column; thin layer Chromatographic, paper S ot tests C%omatographic, thin layer Microcrystallographic S ot tests olumetric, acid-base, nonaqueous Chromatographic; colorimetric Chromatographic; spectrophotometric Chromatographic, gel Chromatographic, paper Chromatographic thin layer Distribution coedcients, ion exchange gels Spectrophotometric, infrared Spectrophotometric, ultraviolet
vp
Papaverine derivatives
Papaver somniferum alkaloids Porphyroxine Protopine Salsolidine Sa1so1ine
Tazettine Thebaine
Isoquinoline, bis-benzyl alkaloids Emetine Ipecacuanha alkaloids
Reference
(1930,8008) (16.91, 1960)
!%);68) (1886, 1930, 1993, ,9008) (636, 968, 1681, 1960, 8807) (96.9. 8316) (668) (1995) (606, 607) (1307) (607) '
(8008)
(938)' (1960, 8836) (1777) (1681)
K(1614, f )1787)
(636, 1614, 1960, 8184, 8 0 8 ) (667) (1681) (1634)
[:gi,
877) flL18. 18861 (1687; 199i,' 8008, 9,989) (636, 788, 1071, 13B7, 1339, 1681, 1809, 1916, 1960, ,9013, 8111, ,9807, 8889) (1188)
(607,1016, 8111) (8889) (3401877) (637) (881, 1,983) (96L (9189 (199Sj (8889) (1993, 2889) (1633) (8,989j
vp
Chromatographic, ion exchange Chromatographic, thin layer Volumetric, ion-pair Tubocurarine Batch ion exchange Chromatographic; electrophoretic Chromatographic, paper; colorimetric Chromatographic; microcrystallographic Analysis of pharmaceuticals in biological media. (Continued on next page)
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
211 R
Table I. Alkaloids (Continued) Compound or Class Pyridine alkaloids Lobelia alkaloids Lobeline
Pyrroliaidine alkaloids General Plat yphylline Quinoline alkaloids Cinchona alkaloids
Cinchonidine
Cinchonine
Dicinchoninic acid Hy droquinidine Hydroquinine Quinidine
Quinine
Method or Subject
Reference
Volumetric, acid-base, nonaqueous Chromatographic, ion ekchange paper Chromatographic, thin layer Oscillopolarographic Spectrophotometric, ultraviolet Volumetric, conductometric
14%
Colorimetric Dialysis Colorimetric Microcrystallographic Volumetric, acid-base, nonaqueous
(184, 1289) (1082)
Chromatographic, thin layer Dialvsis Extractive Extractive, effect of surfactants Ion exchange resin exchange rates Review Spectrophotometric, ultraviolet Spot tests Volumetric, acid-base, nonaqueous Chromatographic, paper Chromatographic, thin layer Ex tractive Spectrophotometric, ultraviolet Chromatographic, paper Chromatographic, thin layer Spectrophotometric, infrared; extractive Spectrophotometric, ultraviolet Ultrasonic degradation Volumetric, acid-base, nonaqueous Polarographic Spectrophotometric, ultraviolet Chromatographic, thin layer Spot tests Volumetric, ox.-red. Chromatographic, thin layer S ot tests olumetric, ox.-red. Chromatographjc Chromatographic, ion exchange Chromatographic, thin layer Fluorometric Gravimetric Hydroquinidine in ; volumetric, ox.-red. Identification Ionization phenomena Luminescence Spectrophotometric, ultraviolet Stability Volumetric, acid-base, nonaqueous Volumetric, ox.-red. Chromatographic Chromatographic, paper Chromatographic, thin layer
.sp
Differential thermal analysis Extractive, effect of surfactants Fluorometric Hydroquinine in; chromatographic, thin layer Hydroquinine in; volumetric, ox.-red. Ionia at ion phenomena Luminescence Spectrophotometric, ultraviolet S o t tests ltrasonic degradation Volumetric, acid-base, nonaqueous Volumetric, complexometric Volumetric, photochemical; fluorometric S ectrophotometric, infrared CP,romatographic, paper Electrophoretic Oscillopolarographic; polarographic
(226, 966) (1637) (2966)
(1697)
(mr)
(240,663, 1418, 1616, 2320) (7,346, 430, 1676,1~77,19m, ~063, 2236) (744) (497) (619, 1161) (1676) (1697)
rp
Quinine ethyl carbonate Quino toxin Steroidal alkaloids Lycopersicon esculentum Solanaceae alkaloids
Colorimetric; gravimetric Chromatographic, gas Chromatographic, paper; densitometric Chromatographic, thin layer
(881) (1209) (2066)
(1616)
(2116) (2186) (1069) (894)
Analysis of pharmaceuticals in biological media. (Continued on next page)
212 R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
Compound or Class Solanum alkaloids Solasodine Tomatine Tropane alkaloids Anisotropine methobromide Atropine
Belladonna alkaloids
Cocaine Homatropine
Hyoscine Hyoscyamine
Methylatropine bromide Scopolamine
Tropeines Tropine Xanthine alkaloids Caffeine
Table 1. Alkaloids (Continued) Method or Subject Chromatographic, paper; densitometric Chromatographic, thin layer Colorimetric, complexometric ion-pair Chromatographic; colorimetric Extractive; volumetric, acid-base Colorimetric; gravimetric
Reference (1069) (598, 1758) (18Y, 398)
(398) (2016) (2116)
Colorimetric, ion-pair Chromatographic Chromatographic, column Chromatographic, gas Chromatographic, ion exchange Chromatographic, paper
( 1683B) (2173)
Chromatographic, thin layer
(194, 246, 284, 541, 342, 468, 1071, 1171, 1424, 1781, 1961, 8013, 8089, 8236) (,w,8 4 4 , i i ~ i ii76, , 1424, ,mso) (1889. 2076) (744)' (L97I
Colorimetric Densitometric Differential thermal analysis Extractive; effect of surfactants Fluorometric Gravimetric Identification Micro crystallographic Spectrophotometric, infrared Spectrophotometric, ultraviolet Stability Volumetric, acid-base, nonaqueous Volumetric, amperometric Volumetric, com lexometric Volumetric, conauctometric Chromatographic, column Chromatographic, paper Chromatographic, thin layer Densitometric Extractive; comparative study Extractive; effect of surfactants Pharmacopoeial: isolation, identification, analysis Volumetric, acid-base, nonaqueous Chromatographic, thin layer Microcrystallographic X-ray diffraction Chromatographic, gas Chromatographic, thin layer Volumetric, acid-base, nonaqueous Volumetric, ox.-red. Chromatographic, paper Chromatographic, thin layer Determination Chromatographic Chromatographic, gas Chromatographic, paper Chromatographic, thin layer Colorimetric Densitometric Determination Ethylene oxide effect on Polarimetric Volumetric, acid-base Volumetric, acid-base, nonaqueous Volumetric amperometric Neutron activation analysis Chromatographic Chromatographic, gas Chromatographic, paper Chromatographic, thin layer Colorimetric Densitometric Extractive; effect of p H Volumetric, acid-base, nonaqueous Chromatographic, thin layer Chromatographic, column Chromatographic, thin layer Volumetric, microconductometric
Automatic analysis Chromatographk, gas Chromatographic, ion exchange Chromatographic, paper Analysis of pharmaceuticals in biological media.
(881)' (2870, 2871 ) (938) (1886, 2076, 2307) (96, 938, 1387, 1662, 1886, 2236) (1886, 2076) (296, 1663) (L96I
(326, 2076) ($076) ( 1171, 1961 ) (606)
(2173) (2333I (1664,' 1889, 2076, 2133, i?307) (341, 542,567, 1171, 1662, 1664, 1777, 2013) (542) ' (367, 2889) (606)
(177f) (2173) (887) (8173, 2218) (2096I (831) '
(.u 7.9\
(367) (28) (2173) (2013) (1176) (342, 2013) (2271) (826. 1876)
(Continued on next page)
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
213 R
Compound or Class
Table I. Alkaloids (Continued) Method or Subject Chromatographic, thin layer Colorimetric Complex formation Densitometric Differential thermal analysis Distillation Extractive, countercurrent Extractive; effect of electrolytes Fluorometric Gravimetric Identification, review Melting oint, reference standard Spectropiotometric Spectrophotometric, ultraviolet
Thermal methods Volumetric, acid-base Volumetric, acid-base, nonaqueous Volumetric, ox.-red. Chromatographic, thin layer Theobromine Gravimetric Identification Microcrystallographic Spectrophotometric, ultraviolet Volumetric, argentometric Volumetric, conductometric Volumetric, ox.-red. Chromatographic, gas Theophylline Chromatographic, thin layer Complex formation Differential thermal analysis Electrodialysis Gravimetric Identification, review Microcrystallographic Spectrophotometric, ultraviolet Thermal methods Volumetric, acid-base, nonaqueous Volumetric, argentometric Volumetric, conductometric Volumetric, ox.-red. Chromatographic, gas Xanthine, general Chromatographic, ion exchange Chromatographic, paper Chromatographic, thin layer Complex formation Identification, review Mass spectrometric RiIicrocrystallographic Spectrophotometric, ultraviolet S ot tests olumetric, ox.-red. Analysis of pharmaceuticals in biological media.
vp
Table 11. Antibiotics Method or Subject Fluorometric Spectrophotometric, ultraviolet Electrophoretic Aminosidin Stability Amphotericin Chromatographic, ion exchange Antibiotics, general methods Chromatographic, thin layer Disintegration test Electrophoretic Identification Polarographic, review Review, methods Solubility in 26 solvents S ectrophotometric, ultraviolet $olumetric, acid-base Volumetric, ox.-red. Antimycin Fluorometric Stability Aureofungin Stability Bacitracin Chromatographic, paper; thin layer; electrophoretic Capreomy cin Chromatographic, thin layer Carbomycin Chromatographic, thin layer Analysis of pharmaceuticals in biological media. Compound or Class Actinomycins
214R
ANALYTICAL CHEMISTRY, VOL. 43,
NO. 5, APRIL 1971
Reference
(608j )
(2313) (1849; 1982, 2064, 8339) (46.2, 1663) (698, 1206,1662, 1653, 1900, 1991, $013) (1990) 11988) (1613,’ 1641 ) (698, 1014, 1016) (1990) (1864) (1663) (613)
(598. 1206. 1633, 1809, 1990, 1991, 2013)
(698, 1014) (886) (466)
(614, 2264) (1664) (1663, 2189) (32, 26.2) (1707) (1992) (1206, 1663, 1987, 1991, 2013, 2.288)
t$%) [%Si (6.21,1014) (2288)
(1663, 1666)
Reference (67SB) (206)
[KL)
(1868) (81, 1282, 1.401) (661) (1234) (BB39) (1101) (664, 1816) (1266) (206)
(1746) (6691 (1831)
KL) (1984) (6196) (1448)
(Continued on next page)
Table II. Compound or Class Cephalosporins
Antibiotics (Continued)
Method or Subject Chromatographic, thin layer Colorimetric Polarographic Chromatographic, paper Chloramphenicol Chromatographic, thin layer Colorimetric Crystallographic Hydrogen number Identification, spot test Mass spectrometric Polarographic Spectrophotometric, infrared Volumetric, ox.-red. Volumetric, precipitation Chromatographic, paper Chlortetracycline Chromatographic, thin layer Crystallographic Stability Automatic analysis Colistin Chromatographic, thin layer Cyanomycin Chromatographic, thin layer Cycloserine Electrophoretic Stability Volumetric, acid-base Stability Desertomycin Des tomycin 0 tical rotatory dis ersion Doxycycline Cgromatographic, t f i n layer Erythromycin Chromatographic, thin layer Crystallographic SDectroDhotometric. ultraviolet Filipin Sbbilit'y Furacilin Colorimetric Gabbromycin Electrophoretic Gentamicin Chromatographic, paper Chromatographic, thin layer Electrophoretic Hamycin Stability Hygromy cin Colorimetric Optical rotatory dispersion S ectrophotometric, ultraviolet Kanamycin C\romatographic, thin layer Electrophoretic Levorin Stability Lincomycin Chromatographic, gas Chromatographic, thin layer Methacycline Chromatographic, thin layer Narbomycin Chromatographic, thin layer Neomycin Colorimetric Stability Nifimycin Chromatographic, paper Nogalamycin Stability Nystatin Chromatographic, thin layer Oleandomycin Chromatographic, paper Chromatographic, thin layer Colorimetric Stability Olivomycin Chromatographic, thin layer Colorimetric Spectrophotometric, ultraviolet Oxytetracycline Chromatogra hic, thin layer Cr yst allograpiic Spectrophotometric, ultraviolet Stability Volumetric, acid-base Paramomycin Electrophoretic Penicillins Chromatographic, paper Chromatographic, thin layer Colorimetric Countercurrent distribution Dialysis Spectrophotometric, ultraviolet Stability Volumetric, acid-base Volumetric, ox.-red. Polymyxins Chromatographic, ion exchange Chromatographic, thin layer Rifamycin Chromatographic, thin layer Colorimetric Ristomycins Chromatographic,. gas; thin layer Spectrophotometric, infrared Rubomycin Electrophoretic Polarographic Analysis of pharmaceuticals in biological media.
Reference (179) (1966) (9191 (136, 781) (M6, 753, 1193, 1439, 1767) (1193)
(8% ' (14Ob) (69) (63% (667, 866,8211-8218) (1813) (83-9) (1399) (1899) ($61
W) (638)
(1000) (660,842, 1856) (1288)
(1767) (1448) (889, 318) ($9841 (999) (8161) (1988, 1442) (889) (960) (989) (9884) (938) (233) (839 (14) (1698, 1981) (104) ($884 (993, 1.443) (03.9) (SOB, i86,6ro, 809) (692,670, 809, 1898, 1906,8107,2202) (666,1450) (9107) (493) (96)
(698, 670, 1615, 8884) (1698, 1693) (669, 963)
(890) (868)
(1196) (16,900) (1198) (1198) (1063) (483)
(Continued on nest page)
ANALYTICAL CHEMISTRY, VOL. 43,
NO. 5, APRIL 1971
215
R
~
Compound or Class Siccarin Streptomycin
Thiamphenicol Trichomycin Tyrothricin Viomycin
Table II. Antibiotics (Confinued) Method or Subject Chromatographic thin layer; colorimetric Chromatographic: ion exchange Chromatographic, paper Chromatographic, thin layer Electrophoretic Fluorometric Polarographic Stability Volumetric, ox.-red. Volumetric, ox.-red. Automatic analysis Chromatographic, gel Chromatographic, paper Chromatographic, thin layer Colorimetric Crystallographic Fluorometric Partition coefficients Spectrophotometric, ultraviolet Stability Chromatographic, thin layer Spectrophotometric, infrared Stability Colorimetric Chromatographic, thin layer Colorimetric Electrophoretic
Reference (66) (641, 1109) (806) (982, 8196) (980-982)
(697,’ 633, 717, 819, 2800) (42, 764, 1191, 1193, 1282, 1430, 1449, 1902, 2164, 8166) (348, 461, 819, 1191, 1193, 1430, 1906) (1622) (1390; 2144) (372) (461; 1666) (633, 764, 819) (763, 1702) (1702)
Table 111. Inorganic and Metal-Organic Compounds Method or Subject Reference Volumetric, complexometric (112, 113, 237, 2183) ($241 Atomic absorption Atomic absorption (1304) Colorimetric (1943) Arsenic Colorimetric (448, 1814) Identification Volumetric, ox.-red. Ashing (1931) Arsenic, organic Chromatographic, paper (1632) Identification (910) Spectrophotometric, ultraviolet Stability Volumetric, precipitation (718) Barium Atomic absorption Gravimetric Bismuth Gravimetric (1894) Volumetric, complexometric (237, 2110, 2116) Boric acid Volumetric, acid-base (616) Bromides Volumetric, precipitation (1074) Chromatographic, paper; thin layer (7998) Bromine, organic Neutron activation analysis (1912) Radiometric (803) Volumetric, complexometric X-ray emission Atomic absorption (163, 370) Calcium Colorimetric (303) Gravimetric Volumetric, complexometric Volumetric, coulometric Volumetric, ox.-red. Chlorides Gravimetric (789)’ Refractometric Volumetric, precipitation (1211 Chlorine, organic Colorimetric 2164) Identification (1912) Neutron activation analysis Spectrophotometric, flame (1861) Volumetric, complexometric (465, 884) Volumetric, precipitation (1944) Cobalt Chromatographic, ge! (1126) (687, 688, 1261) Chromatographic, thin layer (688, 977) Colorimetric Polarographic (1379) Copper Chromatographic, gel (1126) (688, 1261 ) Chromatographic, thin layer (688, 977, 1667) Colorimetric Cyanides Colorimetric (2080) Electrochemical (963) Analysis of pharmaceuticals in biological media. Compound or Class Aluminum Ammonia Antimony
[%;A)
‘c:Zb) [E;:;io)
;;;:i;
[p?)
(Continued on next page)
216R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
~
Table 111. Inorganic and Metal-Organic Compounds (Continued) Compound or Class Method or Subject Reference Fluorides Ion-specific electrode (1868) Neutron activation analysis (878B) Fluorine, organic Chrometographic, gas (1694) Colorimetric (1944) Volumetric, complexometric (1841) Gold Atomic absorption (1980, 81049 Colorimetric (906,8267) Inorganic, general methods Atomic absorption (1166) Colorimetric (314, 10268, 1626) Emission spectrographic (94) Identification (1086B) Isotope dilution; molecular sieve (818) Neutron activation analysis (1888) Spectro hotometric, infrared, (1666) of haggenated compounds Tetraphenylborate, use of, review (8138) Volumetric, complexometric (1076) Iodides Ion-specific electrode (893) Neutron activation analysis Volumetric, ox.-red. 1114) Photon activation analysis Iodine (8708, 871, 8 W B ) Volumetric, ox.-red. (885) Volumetric, precipitation (1338) Iodine, organic Chromatographic, pa.per (88, 2177) Chromatographic, thin layer (88) Colorimetric Identification Radiometric (416, 838) E$ectrophotometric, flame (1861) olumetric, complexometric (884, 1604) Volumetric, ox.-red. (888, 883, 1094, 1144, 1944) Atomic absorption Iron Chromatographic, gel Chromatographic, thin layer (1261) Colorimetric (172, 448, 916, 9.97, 977, 1184) X-ray emission (172) Lead Neutron activation analysis (8789 Volumetric, complexometric Lithium Atomic absorption 8882B) Magnesium Volumetric, complexometric (118, 113, 839, 491, 1017) Volumetric, coulometric (663) Manganese Chromatographic, thin layer (688, 1261) Colorimetric (448, 688) Emission spectrographic (678) Mercury Chromatographic, thin layer (1878) Identification (8180) Neutron activation analysis Ashing Mercury, organic ) Chromatographic, gas (14899) Chromatographic, paper (1638) Chromatographic, thin layer (761, 8896) Colorimetric (1467, 1874, 9084) Identification (8180) Polarographic (1637) S ectrophotometric, ultraviolet (1632) Qolumetric, complexometric Metal oxides Chromatographic, thin layer Neutron activation analysis (179gB) Volumetric, ox.-red. Molybdenum Colorimetric Nickel Chromatographic, ge! (1186) Chromatographic, thin layer (688, 1861) Colorimetric (688) Nitrogen, organic Volumetric, acid-base (719) Volumetric, ox.-red. (77) Nitrogen oxides Electrometric (366) Nitroprussides Colorimetric (1870) Peroxides Colorimetric Stability Volumetric, ox.-red. (1966) Phosphates Chromatographic,. paper (449) Mass spectrometric (2043) Volumetric, complexometric Volumetric, precipitation ) Phosphorus, organic Colorimetric (448, 18888) Volumetricl ox.-red. (1841) Potassium Colorimetric (997) Identification (667, 680) Ion-specific electrode (893,984 1 Review, methods (1661) Volumetric, precipitation (6.97, 1768) Selenium Colorimetric (10.94) Analysis of pharmaceuticals in biological media.
if;!,)
i%h
$EA)
tf%,
[fk2
i%)
KL) [;i::{
!E2
(Continued on next page)
ANALYTKAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
217 R
Table 111. Compound or Class Silicon Sodium Sulfates Sulfides Sulfur Sulfur, organic
Thorium Water
Compound or Class Acridines
Amides
Inorganic and Metal-Organic Compounds (Continued) Method or Subject Reference Atomic absorption (1386) Colorimetric (370) Gravimetric (113) Ion-specific electrode Spctrophotometric, flame ) (1363) olumetric, precipitation Identification (1801) Volumetric, precipitation (1073) Colorimetric (1831,1243,2164) Volumetric, complexometric (682,1841) Volumetric, coulometric (878) Volumetric, precipitation (1944) Volumetric, ox.-red. Neutron activation analysis [%B) Chromatographic, gas (974) Electrometric (28%) Gravimetric (134) Review, methods (17.86) f&ectrophotometric, infrared (1907,2234) ermometric (38) Volumetric, ox.-red. (396,668,2079)
[Z
Table IV. Nitrogen-Containing Compounds Method or Subject Colorimetric Fluorometric Identification S ectrophotornetric, visible &lumetric, acid-base Volumetric, amperometric Chromatographic, column Chromatographic, gas Chromatographic, ion exchange Chromatographic, thin layer Collaborative study Colorimetric Determination of impurities in Differential thermal analysis Electrophoretic Gravimetric Identification Spectrophotometric, infrared Spectrophotometric, ultraviolet Stability Volumetric, acid-base Volumetric. ox.-red. Volumetric; precipitation
Reference (663,888) (mr,1724) (1422) (2192) (669) (1632) (1068,2006) (316, 436,829,1030B, 1031B, 1061, 1068,171d B ) (601,1362) (106,676,679,739,760,768,1011, 1030B,1031B,1681,1680,1732,1808, 2011,2171) (1198) (102,492,80XB,818,846,1164,1362, 2048,2060,2182) (63) (886) (168gB)
(2010) (468, 1964,2010, 2273, 85'29) (2329)
Amines Alicyclic amines
Chromatographic, gas Colorimetric Extractive Identification Chromatographic, gas Aliphatic amines Chromatographic, ion exchange Chromatographic, paper Colorimetric Separation Volumetric, acid-base Volumetric, complexometric Volumetric, coulometric Aminosalicylic acids Chromatographic, thin layer Enzymatic Fluorometric Identification Spectrophotometric, visible Stability Volumetric, acid-base Volumetric, ox.-red. Antihistamines Chromatographic, gas Chromatographic, thin layer Colorimetric Identification Microsublimation Polarographic Analysis of pharmaceuticals in biological media.
(300,913, 22278) (2219) (1712B,2006) (286,171I B , 2039) (1398) (940) (1Q 6 i )
(1116) (669)
(iioki107) (634,669,1103-1107,2264) (466.1741) (1196) (896B) (382, (382 1064,1066) (8246,2246,2292) (1623) (1916) (Continued on next page) -
218R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
Table IV. Compound or Class Aromatic amines
Nitrogenous organic bases
Nitrogen-Containing Compounds (Confinued)
Method or Subject Chromatographic, column Chromatographic, ion exchange Chromatographic, paper Chromatographic, thin layer Colorimetric . Electrophoretic Fluorometric Identification Microautoradiographic Polarographic Spectrophotometric, ultraviolet Spectrophotometric, visible Stability Volumetric, acid-base Volumetric, ox.-red. Automatic analysis Chromatographic, gas
Reference (634B) (27rB,601) (1044) ( 1986) (18, 1746) (30)
(46, 1280B) (942, 1096) (1MOB) 743, 1382) (63qB,
I$;;[
(2010) (565, 1154) (299, Sod, 309, 89gB, 1.413,1492, 1669, 1661, 1807, 2087B, 222rB) (467, 1370) (1089, 1494) (309, 420, 508, 7S1, 864, 1884, 1718, 21 96) (47, 383, 420, 1113, 1365, 1747, 184.6, ,92312 ) ( 1835, 2158) (229, 533, 731, 763, l l 3 4 , 1284, 1318, 1319, 1666, 1567)
Chromatographic, Paper Chromatographic, ion exchange Chromatographic, thin layer Colorimetric Differential thermal analysis Extractive, ion-pair
Phenylalkylamines
Procaine and analogs
Sympathomimetic amines
Fluorometric Identification Photochemistry, review Polarographic Review Spectrophotometric Spectrophotometric, ultraviolet Spectrophotometric, visible Stability Tetraphenylborate, use of, review Volumetric Volumetric, acid-base Volumetric, complexometric Volumetric, coulometric Volumetric, ion-pair Volumetric, ox.-red. Volumetric, thermometric Chromatographic, gas Chromatographic, ion exchange Chromatographic, thin layer Colorimetric Electrophoretic Extractive, ion-pair Identification Polarographic Spectrophotometric, ultraviolet Automatic analysis Chromatographic, gas Chromatographic, thin layer Collaborative study Colorimetric Densitometric Extractive, ion-pair Fluorometric Identification Official method Polarographic Review, methods Spectrophotometric, infrared Stability Volumetric, acid-base Volumetric, ox.-red. Automatic analysis Biological Chromatographic, adsorption Chromatographic, gas
Chromatographic, Chromatographic, Chromatographic, Chromatographic,
ion exchange paper partition thin layer
Collaborative study Analysis of pharmaceuticals in biological media.
(608)
*
(486B11860, SO4l, 2293, 2294) (1698) (1485, 2196) (417, 509, 1121) (3359 (146, 209, 420, 1064) (909) (1411) ( 1525) (1154) (37, 339, 536, 538, 1981, 2218)
[$%B”’)
(33,377, 441) (501) (2167) (140, 305, 1867, 227rB) (2229) (362, 1011)
t(11341 $EA)1844, 1974)
(1336, 1704) (1913 ) (147, 1011) (1546) (772, 1031B , 2226) (1279, 1986, 2l2.4,2328) (1099) (1384, 2278) ( 1879) (4,@3,@0) (1088) (2184, 2245, 2246) (8269) (886) (281) (2051) (2188) (426, 2339) (1195, 2179) (510) (1843’) (946B) (101, 230, 2 ~ 5 43OlB, ~ ~ 412, 606, 646, 988, 98gB, 990B, 1168, 1398, 1432, 1672, 2226, 2227B, 2263, 2856, 1163) (770, 810, 96gB, 1249B,1268B,2187B) (13OlB,1722, 1970) (1672) (101, 143B,366, 430B, 460B1596, 646, 909, 96gB, 1160, 1496, 1672, 1706) (1223) (Continued on nezt page)
ANALYTICAL CHEMISTRY, VOL. 43,
NO. 5,
APRIL 1971
219 R
Table IV. Nitrogen-Containing Compounds (Continued) Method or Subject Reference Colorimetric (96gB,96gB, 1163, 126gB, 1626) Densitometric ($66) Electrophoretic (1706) (l373w, 1941B) Extractive Fluorometric (490, 1160, 124gB, 176lB, ~ ? 1 8 7 ~ , 2194, 2217) (60, 696, 1S7SB, 1699, 1703, 1706, 2296) Identification Interferometric (366) Mass spectrometric (1LW Partition coefficients (2io4j Review, chromatographic (2099) Review, methods (490, 1 ~ 5 2 3 ~ ) Spectrophotometric, infrared (412) Spectrophotometric, ultraviolet (640, 1079, 2 2 2 ~ 5 ~ ) Volumetric, conductometric (1260) Automatic analysis (740,'1646) Amino Acids (*922 Chromatographic Chromatographic, column ili88j) (96, 387, 784, 1980B, 2036) Chromatographic, gas (1147, 1362, 1368, 2219) Chromatographic, ion exchange (193. 1287) Chromatographic, paper Chromatographic, thin layer (193; 612, 826, 1363, 1396) Colorimetric (847, 1816, 1263, 1362, 1603) Electrophoretic (1603) Enzymatic (1216) Fluorometric (1471) Identification (1363, 18.45. 2193) Review, methods Spectrophotometric, internal reflectance ( 6 i i )' (1879) Spectrophotometric, ultraviolet Spectrophotometric, visible (2210) Stability (79, 1396) Automatic analysis Amino alcohols (278) Chromatographic, column (1264) Chromatographic, gas (820) (382,1142~) (192h) Chromatographic, ion exchange Chromatographic, thin layer (382, 1264, 1468, 1940, 2046, 2068) Colorimetric (1266) Collaborative study Extraction, ion-pair (948) Fluorometric (11429 Identification (1186) Neutron activation analysis Spectrophotometric, ultraviolet Stability Volumetric, acid-base Chromatographic, paper Amino esters Colorimetric Extractive, ion-pair Identification (148, i200, 1636) Spectrophotometric, ultraviolet (616, 1200) Volumetric, acid-base Volumetric, argentometric (6641 (866, 1196) Volumetric, ox.-red. Automatic analysis Amino ethers (106, 673, 2071) Chromatographc, gas Colorimetric (1267) Fluorometric Spectrophotometric, ultraviolet Stability Chromatographic, paper Amino phenols Chromatographic, thin layer Colorimetric Spectrophotometric, ultraviolet Stability Colorimetric Aziridines Extractive, ion-pair vctrophotometric, ultraviolet olumetric, acid-base Volumetric, coulometric Spectrophotometric, visible Azo Automatic analysis Barbiturates Chromatographic, adsorption Chromatographic, dry column (32,41, 13P, 196, BidB, 262, 378, 412, Chromatographic, gas 413, 723, 897B, 89gB, 1162, 1230B, 1414, 161SB, 1 ~ 5 1 41893) ~, (63gB) Chromatographic, paper (93, 132, 368, 410, ~ $ 3 9603, ~ ~ 63gB, Chromatographic, thin layer 674B, 101gB, 1168, 1260, 1470B, 1614, 1826, 1918, 2026, 2328) (1223) Collaborative study Analysis of pharmaceuticals in biological media. (Continued on nezt page) Compound or Class
[?EA)
220R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
Table IV. Nitrogen-Containing Compounds (Continued) Method or Subject Reference Colorimetric (78, 49gB, 1876, 2063, 2060) Extractive ion-pair (2311 Fluorome t Eic (2311 Gravimetric (113) Identification (46, 257, 338, 393,48gB, 50OB,677, 769, 788B, 1302, 1373B, 1394, 1414, 1917, 1983) Microcrystallographic (482, 1203) Polarographic (2017) Proton magnetic resonance (89, 201 7 ) Review, methods (110, 1309) Review, stability (217) Spectrophotometric (266, 1190, 2333) Spectrophotometric, infrared (393,412,413, isoq Spectrophotometric, ultraviolet (287, H O B , 263, 463, 621,7%rB,1469B, 1L70B) Stability (444, 948, 1683) Volumetric, acid-base (19, 603, 961, 1492, 1836, 193%) Volumetric, argentometric (963) Volumetric, complexometric (161, 1332) Volumetric, ox.-red. (962) Volumetric, precipitation ($3461 Chromatographic, gas (30ZB,1230B, 1262) Benzodiazepines Chromatographic, thin layer (758, 2252B) Colorimetric (710, BIOSB) Determination of impurities in (146) Fluorometric (268) Gravimetric (768, (708, 710) 1441, 1734, 2251B) Identification Polarographic (660, 1462-1 466) Review Spectrophotometric, infrared Spectrophotometric, ultraviolet (160B) Volumetric, complexometric (708) Automatic analysis Carbamates (Lo6) Chromatographic, ga? (323,' 484, 486B, 89BB) Chromatographic, thm layer (778) Colorimetric (249, (249; 2130) Spectrophotometric, infrared (1871) Automatic analysis Dibenzazepines (21. 23) Chromatographc, gas (1896, $242) Chromatographic, paper (l8lSB) Colorimetric (663, 604, 1O2rB, 1816B) Electrophoretic (1817) Extractive, ion-pair (6041 Identification (1027B,2186) Spectrophotometric, ultraviolet (166) Automatic analysis Guanidines Chromatographic, column Chromatographic, paper Chromatographic, thin layer Colorimetric Gravimetric S ectrophotometric, ultraviolet olumetric, complexometric Stability Homopiperazines Chromatographic, adsorption Hydantoin5 Chromatographic, g&s Chromatographic, thin layer Colorimetric Identification (769, l i 9 4 , 1629, 2326) Review, methods (817 ) Spectrophotometric, ultraviolet (221, 463, 146gB,2221B) Turbidimetric (243) Volumetric, acid-base Hydrazides Colorimetric Hydrazines Gasometric (327) Identification (363, 760) Volumetric, acid-base (617) Imidazoles Chromatographic, ion exchange (841 Colorimetric (1196, 2070) Identification (343, 1966, 1967) Spectrophotometric, ultraviolet (1848) Volumetric, acid-base (901, 2123) Imidazolines Chromatographic, ga? (1340) Chromatographic, thin layer (1666) Colorimetric (1610, 1611) Fluorometric ( 1376) Identification (676, 1187, 1609) Spectrophotometric, ultraviolet (621, 649, 1666) Stability (1544) Analysis of pharmaceuticals in biological media. Compound or Class
((E3)
vp
gl6l?'
(Continued on next page)
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
0
221 R
Table IV. Nitrogen-Containing Compounds (Continued) Compound or Class Indoles
Method or Subject Chromatographic, gas Chromatographic, thin layer Colorimetric Fluorometric Identification Indolineones Volumetric, acid-base Morpholines Identification Spectrophotometric, ultraviolet Stability Volumetric, acid-base Volumetric, ox.-red. Nitriles Chromatographic,. gas Nitro Automatic analysis Chromatographic, gas Chromatographic, thin layer Identification Spectrophotometric, ultraviolet Stability Turbidimetric Volumetric, acid-base Nucleosides Chromatographic Chromatographic, column Chromatographic, @;elfiltration Chromatographic, ion exchange Chromatographic, paper Electrophoretic Enzymatic Spectrophotometric, internal reflectance S ectrophotometric, ultraviolet Oxazolidinones C%romatographic, thin layer Colorimetric Densitometric Spectrophotometric, ultraviolet Stability Volumetric, ox.-red. Phthalazines Identification Microcrystallographic Polarographic Volumetric, complexometric Volumetric, ox.-red. Gravimetric Piperazines Spectrophotometric, ultraviolet Stability Volumetric, acid-base Volumetric, argentometric Volumetric, precipitation Chromatographic, gas Piperidines Chromatographic, ion exchange Chromatographic, thin layer Colorimetric Extractive Fluorometric Gravimetric Identification Mass spectrometric Microcrystallographic Stability Volumetric, acid-base Volumetric, ion-pair Chromatographic, paper Pteridines Stability Chromatographic, ion exchange Purines Chromatographic, thin layer Electrophoretic Enzymatic Fluorometric Identification Spectrophotometric, ultraviolet Volumetric, conductometric Pyrazines Chromatographic, paper Chromatographic, thin layer Identification S ectrophotometric, ultraviolet Qolumetric, complexometric Pyrazoles Identification Stability Volumetric, ox.-red. Pyrazolidines Automatic analysis Chromatographic, thin layer Fluorometric Identification Polarographic Analysis of pharmaceuticals in biological media.
222 R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
Reference (63) (2886) (8286)
(487) (163, 1186, 1188) (1630) (1.483, 1484) (68) (9148) (68) (322, 1486) (466) (566) (8306) (841) (241, 1189, 1194, 1967) (241, 1879) (114) (843) (403, 2183) (612) (1264) (2106) (399, 1248) (23041 (399, 2304) (1898) (618) (1848, 1264) (216) (888)
$Z) ($148) (322) (3641
t%{
(638, 718, 713)
%) (2OO11 (1646)
(80011
%;A)
(1’?14B, 8003B,2866B) (1604) (816’, 344)
(161, 1898) (1897, 1892) (1088) (1602) (1813) (216’)
(1631) (2866)
(1604, 1606) (1897)
t(18.48, %) 2106)
(8202) (30,1899’, 1900B) (1298) (~576~) (1662) (1248, 189gB, 1900’) (1664, 1667) (706) (869) (706, 760) (706) (869) (1438-1 440) (122) (1440) (28)
(144, 381) (321) (696, 767, 1607, 8190, 2191)
(644) (Continued on nezt page)
Compound or Class
Pyrazolines Pyrazolones
Table IV. Nitrogen-Containing Compounds (Continued) Method or Subject Reference Spectrophotometric, ultraviolet (144, 1180, 1607, 1608, ZZ24B) Stability (144, 321, 1539-1541) Volumetric, ox.-red. (123) Electrophoretic (30) Chromatographic, column (422) Chromatographic, ion exchange (2237) Chromatographic, paper (12) Chromatographic, thin layer (311, 362, 861, 1010, 1581) Collaborative study (1099) Colorimetric (65, 123, 228, 311, 340, 931, 984, 1009, 1133, 1939, 2047, 2049,2129) Electrophoretic (30) Fluorometric (1314) Gravimetric (113, 1352, 1790, 2159) Identification (44, 262, 346, 1675, 1808, 2044) (1251, 1451) Polarographic Spectrophotometric, ultraviolet (311, 422, 1010, 1581, 1788, 2237) Stability (13, 386, 1225, 1775, 1963) Volumetric, acid-base (652, 1836, 2158, 2238) Volumetric, complexometric Volumetric, coulometric Volumetric, ox.-red. ( i 5 7 , 6 9 9 , 7 0 0 , ~ 9 iirgo,i796, , 2174, 2175, 2189) Chromatographic, column Chromatographic, gas 26gB, 299, 300, 315, 373, 73SB, 820, 932B) Chromatographic, gel filtration Chromatographic, thin layer 114 Z B ) Colorimetric (39, 102, 195B, 1211, 1311, 1462, 1472, 1787. 1791 ) Enzymatic Extractive, ion-pair Fluorometric (114.2~~ 1827) Gravimetric (2306) Identification (369, 459, 750, r60, 1041, 1091, 1092, 1211, 1369, 1774, 2290, 2326) Polarographic (1997) Review, methods (256)' Spectrophotometric, ultraviolet (657, 1361, 1774, 2248BJ2319) Spectrophotometric, visible (427) Stability (879, 1535, 1542, 1543) Volumetric, acid-base (455,957,17r4,1887) Volumetric, com lexometric (197, 851) Volumetric, confuctometric (1L.21) Volumetric, coulometric (ibrsj Volumetric ox.-red. (6991 Polarographic (1998) Volumetric, ox.-red. (939) Chromatographic, ion exchange (967, 1481) Electrophoretic (189gB,1900B) Gravimetric (1108) Identification (1773) S ectrophotometric, ultraviolet (628, 1248, 1684, 1880, 189gB, 1900B ) olumetric, acid-base (1685)
!;$:A)
Pyridines
igfE!
i%f
Pyridones Pyrimidines
Quaternary ammonium compounds
jP
Automatic analysis Chromatographc, gas Chromatographic, ion exchange Chromatographic, paper Colorimetric Densitometric Extractivet ion-pair Gravimetric Identification Mass spectrometric Microcrystallographic Spectrophotometric, ultraviolet Stability Volumetric, acid-base Volumetric, amperometric Volumetric, argentometric Volumetric, complexometric Volumetric, coulometric Volumetric, ion-pair Quinazolines Identification Quinolines Colorimetric Gravimetric Identification Nitrogen analysis Polarographic Spectrophotometric, infrared Analysis of pharmaceuticals in biological media.
f730B) (917, f330,2120) (1604) (192, 198, 702) (39, 198, 711, 967, 1177, 1481, 1506) (192) (75. 158gB) (1562) ' (479, 579, 580,702, 926, 1501, 1780)
{!EA)
(702, 1506) (590, 1530) (75, 479, 1604, 1505) ( 16398)
(1503)
Kb) (1897)
:;3; (1619)
(1096; 1422, 1619) (1032) (287, 1426, 1588) (1899, 2147)
(Continued on nezt page)
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
223 R
Compound or Class
Tetrazoles
[:E;)
Triazines Uracils Urea and derivatives
Xanthines
Compound or Class Alcohols
Aldehydes Anthraquinones Carboxylic acids and derivatives Aliphatic acids
Aliphatic esters
Anhydrides Aromatic acids
Aromatic esters
Salicylic acid and derivatives
B
Table IV. Nitrogen-Containing Compounds (Continued) Method or Subject Reference Spectrophotometric, ultraviolet (1486) Volumetric, complexometric (642) Volumetric, coulometric y$4) Colorimetric Volumetric, precipitation Extractive, ion-pair Identification (964) Spectrophotometric, ultraviolet (964) Identification (681, 2094B) Volumetric, ox.-red. (746, 1086) Chromatographic, thin layer (678B) Collaborative study (1197) Colorimetric (947, 1018B, 1087) Identification (1629) Chromatographic, gas (262) Review (1988) Volumetric, ox.-red. (1666, 2189) Table V. Oxygen-Containing Compounds Method or Subject Chromatographic, gas Chromatographic, thin layer Colorimetric Distillation Identification Polarographic Refractometric Spectrophotometric, internal reflectance Spectrophotometric, ultraviolet Volumetric, precipitation Enzymatic Polarographic; volumetric, ox.-red, Chromatographic, thin layer Chromatographic, column Chromatographic, gas Chromatographic, ion exchange Chromatographic, paper Chromatographic, thin layer Colorimetric Fluorometric Radiometric Spectrophotometric, infrared S ectrophotometric, ultraviolet &lumetric, acid-base Volumetric, ox.-red. Chromatographic, column Chromatographic, thin layer Colorimetric Fluorometric Spectrophotometric, ultraviolet Stability Chromatographic, thin layer Microcrystallographic Chromatographic, gas Chromatographic, paper Chromatographic, thin layer Colorimetric Identification Spctrophotometric, ultraviolet olumetric, acid-base Volumetric, ox.-red. Aut omat i c analysis Chromatographc, gas Chromatographic, thin layer Colorimetric Polarographc Stability Spectrophotometric, infrared Volumetric, acid-base Chromatographic, column Chromatographic, gas Chromatographic, gel Chromatographic, ion exchange Chromatographic, paper Chromatographic, thin layer
Analysis of pharmaceuticals in biological media.
224R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
Reference (38, 177, 371, 618, 688, 623, 1176, 1726, 1883) (177, 978, 1168, 1918, 2162) (43211140)
(2090) ( 1686) (1139, 1818,2171, 2214) (601, 1961) (346, 666) (601)
(1067, 1120, 2318) (169, 1120) (1099) (1272, 1347, 1918) (106, 8330) (106. 8330) (149) 0 49) (17,148, 1708) (2181 (2181)
(1869j
(1691) (369) (1784) (6& 707, 1481, 1739) (1660. ( 1660, 1772) (109,'148, .81) 148, i2881) (1836, 2064) (1644, 1906) (1646) i;%yi314, 1347, 1806, 1820, 1918, 2286) 2031, 2071) (486, (486, 2031, 2071)
[7%, 2121, 2122) (1099) (663)' (7@, 1169) (1766, 17MB) (1168) (2237)
igii,) 346, 608, 612, 701, 1019, 1080, 1163, 1784) (Continued on next page)
Compound or Class
Table V. Oxygen-Containing Compounds (Continued) Reference Method or Subject Colorimetric (407,662,8060,8338) Dissolution Extractive Fluorometric (788Bi1660) Identification (2283) Polarographic (2067,2069) Spectrophotometric, infrared (433,~ $ 8 9 686, ~ ~701,703,1078,1761B, Spectrophotometric, ultraviolet 1862. 1864.2046) X-ray diffraction Stability Volumetric, acid-base Volumetric, precipitation Volumetric, ox.-red. Chromatographic, thin layer iiosi ‘ Colorimetric Polarographic Spectrophotometric, ultraviolet Stability Volumetric, acid-base Chromatographic, paper Chromatographic, thin layer (824,960B,978) 12136) Colorimetric (iSS4,’ 19i4~, 232s) Polarographic (1046,1303,1386) Spectrophotometric, ultraviolet Volumetric, complexometric (164, (841)283,446-447,1240,1316,1474, Chromatographic, gas 1829,1832, 8083, 2149) (1837) Chromatographic, paper Chromatographic, thin layer
%%
C hromones
Coumarins
Essential Oils
Ethers
Furans
Furocoumarins Glycosides Anthraquinones
Cardiac
Digitalis
Flavone
B
Colorimetric Distillation S ectrophotometric, ultraviolet C\romatographic, gas Chromatographic, paper Chromatographic; spectrophotometric Chromatographic, thin layer Fluorometric Nuclear magnetic resonance Polarographic Spectrophotometric, ultraviolet Volumetric, acid-base Chromatographic, paper Chromatographic, thin layer Colorimetric Identification Spectrophotometric, ultraviolet Chromatographic, paper Chromatographic, thin layer Chromatographic, column Chromatographic, gel Chromatographic, pa.per Chromatographic, thin layer Colorimetric Identification Review, methods Stability Chromatographic, gas Chromatographic, paper Chromatographic, thin layer Colorimetric Polarographic, review Chromatographic, column Chromatographic, gas Chromatographic, paper Chromatographic, thin layer Colorimetric Enzymatic Fluorometric Microcrystallographic Radiometric Review Spectrophotometric, infrared Chromatographic, column Chromatographic, paper Chromatographic, t h n layer
Colorimetric, Fluorometric Spectrophotometric, ultraviolet Analysis of pharmaceuticals in biological media.
(2166j (164,122gB) (8,1321, 1616) (380)
(2078) (1867) (380)
(1996) (17) (1673) (136) ($41)
(1221) (2346) (1008,2346) (61,766,1138, 1139, 1221,2346) (64,222, 298, 1008,1168,1476) (2162) (2037) (86) (1290)
(1136) (6i6,978,1436,1437,2202) (1670) (1101) (802)
(2033)
(279,801, 1671,2860) (181,474,802, 1666,1668,1669, 1671, 183fIB,2088) (181,801, 1670,1671,2260) (28gB) (800) (1420)
(611@38, 840,1864,22741 (62,1819,1837,1888) (186,626,824,840,978,1088, 1681, 1837,21 71 ) (222, 1219. 1.469. 2216) (iigi,1888) ’ (1046,117’0,1264)
(Continued on next page) ANALYTICAL CHEMISTRY, VOL. 43,
NO. 5, APRIL 1971
225 R
Compound or Class Miscellaneous
Oligosaccharides
Phenolic
Table V. Oxygen-Containing Compounds (Confinued) Method or Subject Reference Chromatographic, column (1380) Chromatographic, thin layer; radiometric (1806) Colorimetric (261, 1380) Extractive (1058) Refractometric (1628) Spectrophotometric, ultraviolet (1049) Stability (2012) chromatographic, gel (1510) Chromatographic, thin layer (656, 1463, 2524) Colorimetric (52, 656, 908) Electrophoretic (507) Molecular Weight Distribution (1904B) Automatic analysis (566) Chromatographic, column (1058) Chromatographic, gas Chromatographic, gel Chromatographic, paper (1818) Chromatographic, thin layer (578, 1168, 1710) Spectrophotometric, ultraviolet (1098) Volumetric, acid-base 16661 Chromatographic, paper (862j Chromatographic, thin layer (978, 1020, 2171, 2531) Colorimetric (2163) Electrophoretic (1522) Electrophoretic (1322) Spectrophotometric, ultraviolet (87, 1020, 2163) Volumetric, acid-base (852) Colorimetric Extractive Chromatographic, thin layer (394, 2088) Colorimetric (554, 1670) Fluorometric (2181) Stability (738. 2382) Chromatographic, gas Chromatographic, thin layer Colorimetric Identification Photochemical, review Polarographic Volumetric, acid-base Volumetric, bromometric (572) Chromatographic, column (2100) Chromatographic, thin layer; colorimetric (578, 1028) Polarographic (636, 637) Volumetric, acid-base (2025) Chromatographic, column (1785) Chromatographic, ga: (416, 1770, 2135) Chromatographic, thin layer (795, 1288, 1675, 1770, 1966) Colorimetric (1201, 1966) Identification (1324,1642) Polarimetric (1403, 2073) Review, ion exchange (1776) Stability (583, 996, 1600) Volumetric, ox.-red. (378, 1433) Chromatographic, thin layer (1170) Colorimetric (571, 1645, 2038, 2155) Photochemical, review (1698) Spectrophotometric, ultraviolet (1170) Chromatographic, thin layer (1901j Volumetric, ox.-red. (1903) Chromatographic, ga? (836) Chromatographic, thin layer (346, 508, 1019, 1697, 2132) Colorimetric (846, 2081 ) Gravimetric (112, 113) Spectrophotometric, (1188, 2045) Volumetric, ox.-red. (1644) Chromatographic, gas (165B,268B, 324, 373, 535, 605, 1634, 163jB, 2347) Chromatographic, gel (85LB) Chromatographic, paper (13il) Chromatographic, thin layer (326, 359, 419, 481, 567, 641, $30, 1549, 1686. 1821. 2285) Colorimetric (267, $24, 324, 374B, 70?, 80aB, 904,570, 1406, 1645, 1615, 2247, 2285) Gravimetric (119. filS) (112, I1619) Identification (1660, 1615, 2321) (16t Polarographic (11: (118,593) Spectrophotometric, ultraviolet (105, 419,589, 821, 1082, 1550, 1852, (10.
tKA)
Saponins
Squill Strophanthus
Ketones
Lactones
Monosaccharides
Naphthoquinones
Peroxides Phenol et,hers
Phenols
tgzh)
Volumetric, acid-base Volumetric, ox.-red. B
1936) (589, 66 653, 1862) (881, 19U6) 1906)
Analysis of pharmaceuticals in biological media. (Continued on next page)
226R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5 , APRIL 1971
Compound or Class Polyhydric alcohol esters
Table V. Oxygen-Containing Compounds (Continued) Method or Subject Reference Chromatographic, column (319) Chromatographic, gas (24, $19) Chromatographic, paper (8, 1616) Chromatographic; spectrophotometric (320) Chromatographic, thin layer (24, 120,319, 400,552, 599, 1189,1409,
Nuclear magnetic resonance Polarographic Stability Chromatographic, gas Polyhydric alcohols Chromatographic, thin layer Colorimetric Fluorometric Polarographic Review, ion exchange Spectrophotometric, infrared Spectrophotometric, ultraviolet Volumetric, acid-base Volumetric, ox.-red. Polyhydric phenols and derivatives Chromatographic, gas Chromatographic, ion exchange Chromatographic, paper Chromatographic, thin layer Colorimetric
Xanthenes
Compound or Class Adrenocorticals Aldosterone Corticosterone Cortisone Desoxycorticosterone Dexamethasone
Flu0 cininolone Flurandrenolone General
Hydrocor tisorie
Paramethasone Prednisolone Prednisone Pregnenolone Triamcinolone Androgens Androsterone
Gravimetric Identification Spectrophotometric, ultraviolet Volumetric, acid-base Volumetric, ox.-red. Chromatographic, thin layer; colorimetric Electrophoretic Fluorometric Radiometric
Table VI. Method or Subject
1812) (32020)
(584) (611)
(716,854,2139, 2236) (716,1994, 2078) (2QSB,431, 1617,2092B) (lOSTB,1220) (775,776) (1776) (1926) (22238) (656, 1573) (160, 244, 1473) (864,1478) (27rB) (920)
(386, 526, 582, 591, 814,919,920,2028, 1649, 2202) (16, 626, 707,814, 919,928, 1028, 1048, 1549, 1572) (1620) (1560) (27rB,581, 591, 1336, 1560)
Ki) (912)
(1908) (912) (1662)
Steroids and Hormones Reference
Chromatographic, thin layer; colorimetric Spectrophotometric, internal reflectance Chromatographic, gas Fluorometric Chromatographic, gas Colorimetric Colorimetric Chromatographic, thin layer Colorimetric Radiometric Spectrophotometric, infrared Stability Chromatographic, thin layer Chromatographic, thin layer Chromatographic, ga: Chromatographic, thin layer Colorimetric Spectrophotometric, ultraviolet Volumetric, acid-base Chromatographic, gas Chromatographic, thin layer Colorimetric Fluorometric Spectrophotometric, ultraviolet Chromatographic, thin layer Colorimetric Chromatographic, thin layer Colorimetric Spectrophotometric, ultraviolet Chromatographic, thin layer Spectrophotometric, internal reflectance Colorimetric
Chromatographic, column Chromatographic, thin layer General Chromatographic, pa er; thin layer Methyltestosterone Chromatographic, cofumn Testosterone Chromatographic, gas Chromatographic, paper Chromatographic, thin layer Analysis of pharmaceuticals in biological media.
(1083) (2216) (1081)
(1083, 1172)
(1172,2141) (688) (210, 625,1341) (291B,867, 1349, l(tOZB, 1700) (1083, lY62?, 1933) 12858) (690, 1083, 1033) (354)
(907) (280)
(728,873, 1762) (6891 (354,695,1701 ) (1769) (1081)
(783) (771) (1647B) (783) (50, 51, 488) (2101) (51,180,220, 771,2165) (Continued on nezt p a g e )
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
227 R
Compound or Class
Estrogens Estradiol
Estriol
Estrone
E thynyles tradiol General
Mestranol
Synthetic estrogens
Miscellaneous Androstene derivatives Bufadienolides Corticotrophin Insulin Ketosteroids
Sapogenins Steroid phosphates Sterols
Thyroxine
Table VI. Steroids and Hormones (Corttjnued) Method or Subject Reference Colorimetric (1m9,2101) Spectrophotometric, infrared (611 Spectrophotometric, ultraviolet (6891 Chromatographic, gas Chromatographic, gel Chroma tographi c, t hin layer Colorimetric S ectrophotometric, ultraviolet CRromatographic, gas Chromatographic, gel Chromatographic, thin layer Colorimetric Chromatographic, gas Chromatographic, gel Chromatographic, thin layer Chromatographic, gas Chromatographic, thin layer Colorimetric Chromatographic, gas Chromatographic, gel Chromatographic, paper Fluorometric Review, methods Chromatographic, column Chromatographic, gas Chromatographic, thin layer Colorimetric Fluorometric Spectrophotometric, ultraviolet Chromatographic, gap Chromatographic, thin layer Colorimetric Polarographic Spectrophotometric, ultraviolet Chromatographic, thin layer Colorimetric Chromatographic, column Chromatographic, gas Stability Automatic anal sis Review, metho& Chromatographic, paper; thin layer Review, methods Stability Chromatographic, column Chromatographic, gas Chromatographic, thin layer Colorimetric Fluorometric Gravimetric Review, automatic analysis Spectrophotometric, ultraviolet Chromatographic, thin layer Stability Chromatographic, ion exchange Spectrophotometric, infrared Chromatographic, column Chromatographic, gas Chromatographic thin layer Volumetric, brodination Chromatographic, gas Chromatographic, thin layer Spectrophotometric, ultraviolet
Progestogens Anagestone Et hynodiol General
Chromatographic, gas Colorimetric Chromatographic, ge! Chromatographic, thin layer Megestrol Chromatographic, column Chromatographic, gas Colorimetric Norgestril Fluorometric Progesterone Chromatographic, gas Chromatographic, paper Colorimetric Fluorometric Identification Spectrophotometric ultraviolet Analysis of pharmaceuticals in biological media.
(517,336)
!%,
317, 1186) (317,1146) (689) (317) (991 (317,164gB) (517) (317) (99) (Sl'?,16PB) (2,2028) (2) (169) (438,1036, 1674) (66L)
(1824,1816) (408) (1191) (1763) (687,689491,1142) (207,1972) (208) (170) (1791)
(779)' (1~?60, 1697) (1560) (1891) (1618) ',%)
(11198) (618) (11198) (408) (1771) (2101) (2009,1101) (1143) (1927) (689)
(Continuedon nezt page)
228R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
Compound or Class Steroids, general methods
Compound or Class Benzothiadiazines
Cyclohexylsulfamates
Disulfides
Mercaptans
Miscellaneous
Phenothiazines
Saccharin Sulfide Sulfonamides
Table VI. Steroids and Hormones (Continued) Method or Subject Reference Chromatographic, adsorption; isotopic dilution Chromatographic, gas (Si,-669, 786, lSOOB, 1606, 1727, 1769, 8167, 2168, 8170, 2178) Chromatographic, gel (11L6) (630)' Chromatographic, paper Chromatographic, thin layer (401, 480, 686, 781, 788, 978, lllWB, 1181, 1188, 1860, 1876B,1674, 1830, 1911B, 8164, 2166, 8802) Identification (867, 1607) (90, 8098) Mass Spectrometric (8883) Polarographic 12017 ) Proton magnetic resonance Review ('1607,' 1696, 8096) Spectrophotometric, infrared (580, 804, 8849, 8860) (1769) Spectrophotometric, internal reflectance Spectrophotometric, ultraviolet (8096j
Table VII. Sulfur-Containing Compounds Method or Subject Chromatographic, thin 1ay er Colorimetric Spectrophotometric, ultraviolet Stability Chromatographic, gas Chromatographic, ion exchange Colorimetric Radiometric Review, methods Stability Volumetric, complexometric Chromatographic, thin layer Chronometric Colorimetric Identification Spectrophotometric, ultraviolet Volumetric, ox.-red. Chromatographic, paper Chromatographic, thin layer Fluorometric Polarographic Volumetric, coulometric Chromatographic, thin layer Colorimetric Extractive, ion-pair Identification Polarimetric Polarographic Spectrophotometric, ultraviolet Volumetric, conductometric Volumetric, ox.-red. Automatic analysis Chromatographic, gas Chromatographic, ion exchange Chromatographic, thin layer Colorimetric Determination of impurities in Extractive, ion-pair Fluorometric Identification Partition coefficient Review, methods Spectrophotometric, ultraviolet Stability Volumetric, acid-base Volumetric, complexometric Volumetric, conductometric Volumetric, ion-pair Volumetric, ox.-red. Determination of impurities in Extractive, ion-pair Chromatographic, thin layer Spectrophotometric, ultraviolet Chromatographic, column Chromatographic, gas Chromatographic, paper Chromatographic, thin layer
Analysis of pharmaceuticals in biological media.
Reference
(BoorB)
\?E$; 80079 (1699-2301) (843, 1958B) (1293) (986) (19S8B) (1716)
(208, 219-l)
(376, 450, 84gB, ( 2 1 9 B , 475, 981, (1636)
774B1
581, 1666)
(Continued on next page)
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
229R
Compound or Class
Sulfones Sulfonium salts
Sulfonyl ureas
Sulfophthaleins Sulfoxides Thiazoles Thioamides Thioamino acids Thiobarbituric acids Thioimidazoles Thiosemicarbazones
Thio TEPA Thiouracils Thioureas Thioxanthines
Compound or Class Oil-soluble Vitamin A
Vitamin D
Table VII. Sulfur-Containing Compounds (Continued) Method or Subject Reference Colorimetric (43, 56ZB,620B,943, 1391, 1461, 1768, 1783, 1803, 1804B, 1975) Electrophoretic (1687) Fluorometric (2030) Identification (57, 251, 257, 368, 631, 736, 916, 942, 1033, 8230) Nuclear magnetic resonance (1695, 2017) Polarographic (1101, 2283) Radiometric (1802) Spectrophotometric, ultraviolet (360, 900, 915, 146rB, 1728, 1783, 2032, 2228. 2276) Spectrophotometric, visible (64, lk22) ‘ Stability (735, 2336) Volumetric, acid-base (245, 1531, 1629, Z Z d l , 2339) Volumetric, coulometric (664, 1526, 2209) Volumetric, ox.-red. (865, 1195, 2179) Identification (583) Stability (530, 331) Chromatographic, thin layer (1366) Colorimetric (1366 ) Spectrophotometric, ultraviolet (1366) Spectrophotometric, visible (1084B) Volumetric, ox .-red. 112828) Chromatographic, column Chromatographic, ga; Chromatographic, thin layer Colorimetric Spectrophotometric, infrared Volumetric, acid-base Volumetric, complexometric Chromatographic, thin layer Spectrophotometric, infrared ill8i Volumetric, ox.-red. (147be) Nuclear magnetic resonance (1093) Polarographic (1636) Spectrophotometric, ultraviolet (1865) Chromatographic, gas (1797) S ectrophotometric, ultraviolet 11633) dlumetric, coulometric Colorimetric Electrophoretic St ability Spectrophotometric, ultraviolet Colorimetric Gravimetric Spectrophotometric, ultraviolet (1427,’ 2306) Volumetric, acid-base (2329) Volumetric, complexometric (70.9 Volumetric, precipitation Colorimetric Volumetric, acid-base Volumetric, coulometric Identification (2118) Volumetric, amperometric (556) Identification Chromatographic, thin layer Fluorometric Spectrophotometric, ultraviolet
Table VIII. Method or Subject
Vitamins
Automatic analysis Chromatographic, column Chromatographic, gas Chromatographic, gel Chromatographic, paper Chromatographic, thin layer iMass spectrometric Polarographic Review Spectrophotometric, ultraviolet Spot tests Chromatographic Chromatographic, column Chromatographic, gas
Chromatographic, gel Analysis of pharmaceuticals in biological media.
Reference (56) (49, 631, 1377, 233ZB)
(604, 79gB,905, 1226, 1482, 1856)
(2137) (1226) (9, 49, 397, 531, 793, 79gB,944B, 1226, 1405, 1643, 1717, 2231) (1482) (2161) (443) (1237) (786)
(443,’ 1038) (476, 1039, 1257, 1377) (443, 504, 529, 1377, 1497, 1576, 1606, 1870, 2266, 2308) (2137)
(Continued on nest page)
230 R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
Compound or Class
Vitamin E
Vitamin K
Vitamin P Water-soluble B1, thiamine
Table VIII. Vitamins (Continued) Method or Subject Chromatographic, paper Chromatographic, thin layer Colorimetric Hydrogenation Isomerization Polarographic Review Spectrophotometric, ultraviolet Spot tests Chromatographic, colrimn Chromatographic, gas Chromatographic, gel Chromatographic, paper Chromatographic, thin layer Collaborative study Colorinlet ric Polarographic Review Spectrophotometric, ult raviolet Volumet rir, amperomet ric Chromatographic, gas Chromatographic, thin layer Colorimetric Determination, review Differential thermal analysis Fluorometric Polarographic Spectrophotometric, ul t raviole t l'olumetric, coulometric Fluorometric
.4ut om8 t ic analysis Chromatographic, colurnil Chromatographic, gas Chromatographic, ioii-exchange Chromatographic, paper Chromatographic, thin layer Colorimetric Ex t ract ive Fluoromet yic Gravimetric Ide n t i.fi ca t i o n Kinetic Polarographic Review Spect rophot oniet ric, infrared, of inter mediar e+ Spectrophotometric, iiltraviolet Stability Volunietric, acid-base l'olumetric, amperometric 1701umetric, ion-pair Volumetric, precipitat io11 Bs, riboflavin Chromatographic, column Chromatographic, paper Chromatographic, thin layer Colorimetric Fluoromet riv Identi,fica t ion Kinetic Photochemical Polarographic Review Spectrophotometric; jtability Spectrophotomet ric, ultraviolet Stability BO,pyridoxine .%iiroinaticanalysis Chromatographic, column Chroma t ographir, gas Chromatographic, ion exchange Chromatographic, paper Chromatographic, I hili layer Colorimetric Fluoromet ric Kinetic: enzymatic 1 I u s .spectrometric lieview Spectrophotometric, ultraviolet Spot tests Stability Volumetric, amperometric B Analysis of pharmaceuticals in biological media.
Reference (1576) (565, 777, 795, 1405, 1576, 1577, 1606, 1627, 1717, 2155, 2231) (777, 1039, 1257, 1406, 1576, 1717, 2631) (1237) (996, 1038)
(214, 1039, 1576) (443, 1576, 1596) (365, 1576, 2165)
E!
(443,'905, 1236, 1648, 1869, 1919) (2137) (137) (199,397, 793,813, 1717, 1753,2069) (1869)
(137, 199, 397, 63QB,1372, 1869) (1Ll7) (4i3, 986) (199, 650, 1753) (385) (458, 1895, 2309, 2310) (495, 1170) (2170, 1645)
(1878)
(1408, l76.4) (76) (4, 29, 76, ,307, 1365, 1798) (1046, 1538, 1798) (29, 31, 794, 1277, 1578, 223P) (307, 424, 425, 1271, 1538, 1878) (425)
(875, 892, 1277, 1754, 2302, 2340) (1271)
(402, 2129, 2240) (376B, 1764) (905, 987, 1839)
(1798) (1046, 1100) (si, 442,755, 1277, 1578) (40, 402, 1271, 1750, 2119, 2146) (376B, 1277, 1823) (866, l27SB)
(439B)
(443, 1271)
(1046, 1798, 2001, 2199, 2240) (1211) (1271)
(41 (Continued on nezt p a g e )
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
231 R
Compound or Class B12, cobalamine
B ~ spangamic , acid Biotin C, ascorbic acid
Table VIII. Vitamins (Continued) Method or Subject Volumetric, oscillometric Volumetric, ox.-red. Adsorption, batch Atomic absorption Automatic analysis Chromatographic, column Chromatographic, ion exchange Chromatographic, thin layer Colorimetric Hydroxocobalamine, in Isoelectric focusing Kinetic Radiometric Review; stability Spectrophotometric Chromatographic, paper Chromatographic, thin layer Colorimetric Chromatographic, gas Colorimetric Automatic analysis Chromatographic, column Chromatographic, gas Chromatographic, paper Chromatographic, thin layer Colorimetric Determination; errors from impure carbon dioxide Fluorometric Identification Kinetic Photodecomposition Spectrophotometric, ultraviolet Spot tests Stability, review Volumetric, amperometric Volumetric, ox.-red.
C, fatty acid monoesters Folic acid
Nicotinamide and nicotinic acid
Pantothenic acid
Vitamins, general
Vitamins, general, B-group Vitamins, general, water-soluble
Colorimetric Identification Chromatographic, column Chromatographic, thin layer Decomposition, products of Fluorometric Polarographic Spectrophotometric, ultraviolet Stability Chromatographic, column Chromatographic, gas Chromatographic, ion exchange; paper Chromatographic, thin layer Colorimetric Identification Kinetic Polarographic Review; stability Spectrophotometric, ultraviolet spot tests Automatic analysis Chromatographic, gas Chromatographic, paper Chromatographic, thin layer Colorimetric Kinetic Nuclear magnetic resonance Optical rotatory dispersion Review Spectrophotometric, infrared Chromatographic, thin layer Electrophoretic, thin layer Isotope dilution; molecular sieves Polarographic, review Chromatographic; spectrophotometric internal reflectance Review; stability Chromatographic, thin layer
Analysis of pharmaceuticals in biological media.
232 R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
Reference
(866) (91B,6 0 ~ 51368B, ~ ~ 1698B, 1690B, 209lB) (1271) (1871, 2340) (9949 (2066, 2067) (9948)
(97B, &3, 608, 644, 684, 1169, 1364, 1374, 161S2~,1798, 18HB, 2279) (807)
(464,' 1277, $310) (796, 1042) (866. 867)
(1366) ' (98B,869, 1367, 2111) (1186) (1989) (1239) (332J381, 46% 464, 467, 650, 684, 747, 837, 1374, 1378, 1684, 1719, 1720, 194%) (2128) (2127)
(183, 912, 1160) (76, 906, 987, 1660, 1839) (1798) (31, 384, 469, 1277, 1333, 1678, 1916) (47, 911, 1661) (911, 1661)
g:;)
(1271) (384, 911, 1160, 1271, 1798, 1847) (1211)
(866) (1661) (1005)
'
t$i$l) (1596, 1674) (30) (812) (1101) (612) (986) (978, 2202)
Compound or Clam General methods Aerosols Alkenes Analgesics Anesthetics Anesthetics, loca
Anthracene derivatives Anticholinergics Antidepressive drugs Antihistamines Antiovulating agents Antioxidants Antipyretics Antiseptics Antispasmodics Antituber culars Aromatic systems Azines Benzene chromophores Cardiotonics Carotenoids Cholic acids Cocaine substitutes Curarimimetics Degradation Dienes Drug solution stability Dyes
Enzvmes Gthipsin c Cathepsin D Cellulases, hemicellulases Chymotrypsin Lypolytic activity Pancreas powder Pancreatic enzymes Pancreatin Papain Pepsin Peroxidases Protease inhibitor Pro teinrtses Proteolytic enzymes
Renin Thrombin Trypsin
Fluid extracts General techniques
Table IX. Formulations, Mixtures, and General Methods Method or Subject Reference Chromatographic; colorimetric Chromatogra hic, gas Sampling t ecfnique Photochemical, review Chromatographic, g? Chromatographic, thm layer Chromatographic, gas Chromatographic, gas, review Gas detection membrane Chromatographic, gas Chromatographic, paper; thin layer Chromatographic, thin layer Colorimetric Microcrystallographic Spectrophotometric, ultraviolet Stability, review Chromatographic, thin layer Chromatographic, gas Chromatographic, thin layer Automatic analysis Chromatographic, Microcrystallog r a p t 2 Chromatographic, gas Chromatographic, thin layer Chromatographic, gas Chromatographic, thin layer Review Chromatographic,, gas S ectrophotometric, internal reflectance CPhromatographic, thin layer Chromatographic, gas Photochemical review Chromatographic, thin layer Volumetric, acid-base, nona ueous S ectrophotometric, ultravioqet Ciromatographic, thin layer Chromatographic, thin layer Chromatographic, column; preparative X-ray diffraction Chromatographic, paper; thin layer Review Photochemical, review Review Chromatographic, pa,per Chromatographic, thm layer Electrophoretic, paper Spectrophotometric, internal reflectance
(382)
$%)
(1698) ( 1 4 2 $303) ~~ (1, 96, 1488, 8806, 8303) (38, 290B, 1161, 1888) (2099) (9'76B) (1489 (73'7)
i3Sl
(i084) (666) (82, 14ZB, 89gB)
tf%j
(346,547) (1062, 1346) (1236, 2384) (16'76) (38 (1296) (18277 (300)'
(1698) (1826) (1527)
(2306j (2000) (677B) (i668)' (1698) (8'70,1069) (468-4'70, 8876) (612, 1663, 1674, 1918, 1967, 83.94 1 (471) (612)
Polypeptide digestion ; manometric Automatic analysis Galactomannan digestion Hydroxyethylcellulose digestion; viscorrietric Review Volumetric, formol Olive oil digestion; volumetric Casein digestion; spectrophotometric Hemoglobin digestion Starch digestion Review Casein digestion; volumetric Spot tests, in tragacanth Speqtr ophot omet ric Review Automatic analysis Colorimetric Electrophoretic, starch ge Fluorometric Hemoglobin digestion Review Polypeptide digestion; manometric Review Chromatogra hic, gel column Polypeptide ggestion; manometric Review S ectrophotometric, ultraviolet &lumetric, acid-base Chromatographic, thin layer Fluorometric, review Atomic absorption Automatic analysis
666,
886, 1136,
Analysis of pharmaceuticah in biological media,
(Conhued on nezt page)
ANALYTICAL CHEMISTRY, VOL. 43,
NO. 5,
APRIL 1971
233 R
Table IX.
Compound or Class
Formulations, Mixtures, a n d G e n e r a l Methods (Confinued)
RIethod or Subject Chromatographic, column Chromatographic, column partition Chromatographic, column; preparative Chromatographic, gas
Chromatographie, gas, coupled with mass spectrometer Chromatographic, ion exchange Chromatographic, paper
Reference (361, 1918) (1673) (8305) (32, 94, 14ZB, 14SB, 305, 371, 866, 89gB, 1005, 1058, 1161, 1224, 1328, 1346, 151dB, 1658, 1661, 1673, 1727, 1811, 208YB, 2099, 2150B, 8303, 2324, 2334) (143BI2150B) (877, 1868) (3,8, 467-470, 57TB, 737, 804, 1537, 1971B. 2275)
Chromatographic, review Chromatographic, thin layer
1488; 1496; 151pB,1563, i574, iro6, 1732. 1733. 1735. 1736. 1781. 1788. 1809; 1811; 18866; 1858; 1918; 1945; 1947, 1949, 1967, 1968, 2018, 8084, 2150, 2171, 2208, 2206, 2303, ,8324, 2528)
Chromatographic, thin layer; review Colorimetric Colorimetric, tristimulus Complexometric, review Ilensitometric Dialysis Differential scanning calorimetric Differential thermal analysis Drug availability, review Electrophoretic, paper Emission spectrographic Ex t ract'ive Functional group analysis, review Identification Identification, review Mass spectrometric Mass spectrometric, review Melting point, validation Microchemical hI icrocrystallographic blicroextractive Neutron activation analysis Nuclear magnetic resonance, review Partirle size analysis Partition coefficients Polarimetric Polarographic Polarographic, review Proton magnetic resonance Radiochromatographic Radiometric Refractometric Review Spectrophotometric, infrared Spectrophotometric, infrared Spectrophotometric, infrared, review Spectrophotometric, internal reflectance Spectrophotometric, ultraviolet Spectrophotometric, ultraviolet, automated Spot tests, review Tetraphenyl borate, use of, review Thermal analysis
B
Thermoanalytic, automated Thermomicro analysis Volumetric, acid-base Volumetric, acid-base, nonaqueous Volumetric, amperometric Volumetric, complexometric Volumetric, coulometric Volumetric, ion-pair Volumetric, microcoulometric Volumetric, ox.-red. X-ray X-ray diffraction X-ray diffraction, review Zone melting Analysis of pharmaceuticals in biological media. ~~
234R
0
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
(1968) (740, 763, 814, 101gB, 1145, 1884, 2145, 2312) (508, 979, 1019B, 1070, 151dB, 1524, 1563)
(1559) (257, 467, 737, 1102, 1185, 1559, 1675, lY6L. 1785. 1786. 8293. 2317)
(1124, 1125, 1764, 1785, (Il.%$, 1641, 1973, 2844, 1801i
(i7ik) (1508) (574, 734) (178, 1584) (1016) (613. 8283) (260; 1101)
(2017) (828)' (3, 1282) (1062, 1937) (186, 603, 1594) ($09, 551, 1655, 1788, 1857, 8084) (1295) (647) (612, 1295) (20, 551, 565, 621, l l % 4 , 1125, 11-95, 1793, 1794, 1857, 2084) (565, 1135)
Ki)
(434, 668, 741, 744, 885, 1194, 1834, 1835, 1945, 1947, 8316) (886) (1124, 1125, 1945, 1947) (537, 638, 1154) (37, 1416, 1982, 2818, 8317) (1232) (881, 1145, 8312)
(664, 1525, 1526)
t&A) (452)
(1715) (2000)
(429)
(1291)
(Continued on next page)
Table IX. Formulations, Mixtures and General Methods (Continued) Method or Subject Compound or Class Chromatographic, thin layer Germicides Hallucinogenic drugs Fluorometric Chromatographic, thin layer Hypnotics Chromatographic, paper; radiometric Hypoglycemic agents Chromatographic, thin layer; deterioration Injections Effect on thin layer chromatography Iodine Chromatographic, gas Isopentyloxy groups Laxatives Chromatographic, thin layer Chromatographic, thin layer Naphthalene derivatives (1373*, 1733) Chromatographic, thin layer Narcotics (1373B) Identification Review 1698) Polarographic, review Neuroplegic substances Physicochemical properties Organic complex solutions (949) (979) Chromatographic, thin layer Phospholipids [87l,’1698) Review of transformations Photochemical Polyacet ylenics Chromatographic, paper (1624) (1168) Chromatographic, thin layer Preservatives Chromatographic, thin layer Proteins (2324) (1S73B, 1735, 1812, 2084) Chromatographic, thin layer Psychotropic drugs (139. 313) Stability, review Radiochemicals il729, ’ Chromatographic Radiopaque agents (10951 1729) Spectrophotometric, ultraviolet (1489, 1501) S-ot tests (2171) CPhromatographic, thin layer Resins Analvsis: reactivitv with drum (903) Rubber stoppers Purit;. tests (811) Shellacs (8 Chromatographic, paper Solubilizers (l?27) Chromatographic, gas Solvents Review (1665) Sorption of drugs Chromatographic, thin layer Spermaceti alkyl esters (830) chromatographic, thin layer (1808, 1809, 1811) Suppositories Physicochemical tests (860) Chromatographic, gas 132. 89QB) Sympathomimetics (2305) ’ Chromatographic, column, preparative Tannins Chromatographic, gas (1727) Chromatographic, thin layer Review Thyroid compounds Chromatographic, thin layer (526. 1816) Tinctures Fluorometric, review (626j Chromatographic, gas (89QB) Tranquilizers Identification (137SB) Photochemical, review (1698) Trienes Chromatographic, thin layer (1168) Unsaturated compounds Chromatographic, column, thin layer Wines, medicinal (938) Formulations, mixtures, and miscellaneous Chromatographic, thin layer (1068) Acetaminophen Colorimetric (1164) Differential thermal analysis (744) Identification, review (1675) Spectrophotometric, ultraviolet (540, 1852) Chromatographic, column (1068) Acetaminophen, acetylated Automatic analysis; thermal analysis (885)’ Acetanilide Chromatographic, gas Acetone (607) Chromatographic; spectrophotometric Acetrizoic acid (1729) Chromatographic, gas Acetylsalicylic acid (435) Chromatographic, paper Chromatographic, partition column (346, 612, 1068, 12/30, 1539, 1811, 2206) Chromatographic, thin layer Densitometric (508) Differential thermal analysis (744) Electrophoretic, paper Identification, review W 5 ) Spectrophotometric, internal reflectance (612) Spectrophotometric, ultraviolet (1169) Volumetric, acid-base; weight variation (1060, 1852) Acrinol Spectrophotometric; stability Adiphenine Chromatographic, thin layer Volumetric, acid-base, nonaqueous Chromatographic, gas Adrenaline ($30) Volumetric, conductometric ( 1250) Chromatographic, thin layer Alconium (1780) Chromatographic, thin layer Allobarbital (362, 1781, 1811) Chromatographic, thin layer Allylisopropyl-barbituric acid (1811) Colorimetric; extractive Aloins (1757) Chromatographic, thin layer Amidoantipyrine (1781) Chromatographic, paper p-Aminobenzoic acid (5531 Spectrophotometric, ultraviolet p-Aminohippuric acid (1090)
{j?;],
-
1K%,
Iff%
B
Analysis of pharmaceuticals in biological media. (Continued o n next page)
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
235 R
Table IX. Formulations, Mixtures and General Methods (Continued) Method or Subject Reference Chromatographic, thin layer Fluorometric Stability to infrared radiation Aminophylline Chromatographic, thin la er Volumetric, acid-base, coLrimetric Aminopropylon Colorimetric Aminopyrine Chromatographic, gas (1346,' 2303) Chromatographic, thin layer (96, 946, 101gB, 1661, 1663, 1811, 1916, 2206, 2303) Electrophoretic, paper Extractive; gravimetric Identification, review Microcrystallographic; volumetric i16.61 i Polarographic S ect ropho t omet ric, ultraviolet d h r n e t r i c , acid-base, nonaqueous Amitriptyline Chromatographic, thin layer Densitometric Amizil Volumetric, acid-base, nonaqueous Amobarbital Chromatographic, gas (2166) Volumetric, acid-base, nonaqueous Amphetamine Chromatographic, thin layer Volumetric, conductometric Analgin Chromatographic, thin layer Colorimetric Volumetric, acid-base, nonaqueous Anise Chromatographic, thin layer Antipyrine Chroma tographic Chromatographic, gas Chromatographic, thin layer Fluorometric Identification, review Volumetric Volumetric, acid-base Volumetric, ox.-1ed . Antipyrine derivatives Volumetric, coulometric; microanalysis Apressin Volumetric, acid-base, nonaqueous Aqua menthae piperitae Chromatographic, gas Arnica roots Chromatographic, thin layer Artemsia ketone Chromatographic, paper Atarax P Chromatographic, thin layer Axerophthol Chromatographic; spectrophotometric Azobenzene Chromatographic, thin layer Balsum Peru Chromatographic, gas; thin layer Barbituric acid Electrophoretic, paper Benzacine Volumetric, acid-base, nonaqueous Benzene Chromatographic,. gas Benzocaine Automatic analysis; colorimetric Chromatographic, thin layer (1939; 1809) Microcrys tallographic (2246) Volumetric, amperometric (1232) X-ray diffraction (2000) Benzoic acid Complex formation Betaine Automatic analysis; enzymatic Chromatographic, ion exchange Volumetric, conductometric Bilignost Spot tests Bilitrast Spectrophotometric, ultraviolet Spot tests Br ompheni r amine Colorimetric Cacao butter Automatic analysis; thermal analysis Caffecetin Chromatographic, thin layer Cannabis Chromatographic, column Chromatographic, gas (6Y,' 71, 197, 616, 1167, 1228, 2097) Chromatographic, ion exchange; paper 119YOB) Chromatographic, thin layer (67, 72; 73, 296, 310, 616, 933, 1128, 137SB, 1602) Colorimetric (724) Review (1696) Spectrophotometric, infrared (923) SDectrouhotometric, ultraviolet (724, 933) Spot tests (320, 436, 1194) Carbinoxamine S ectrophotometric, ultraviolet (1361) Carbromal romatographic, thin layer (1809, 1916) Cardiotrast Spectrophotometric, ultraviolet ( 1096) Cassia fistula Chromatographic, thin layer (2236) Castor oil Chromatographic, thin layer (672) Centrine Microcrystalline (8293) Chamomile Chromatographic, thin layer (1946) Chloracizine Chromatographic, thin layer Chlorambucil Spectrophotometric, ultraviolet Analysis of pharmaceuticals in biological media. (Continued on nezt page)
Compound or Class Aminophenazone
CR
236R
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5 , APRIL 1971
Table IX. Formulations, Mixtures and General Methods (Continued) Method or Subject Chromatographic, thin layer Stability Volumetric amperometric Chlordelazine Chromatographic, thin layer; densitometric Chlordiazepoxide Spectrophotometric, ultraviolet Chloridine Chromatographic; colorimetric Chlorocholine Colorimetric, ion-pair Chloro yramine Chromatographic, partition ChlorpReniramine Chromatographic, thin layer Colorimetric Fluorometric Volumetric, complexometric Chromatographic, thin layer Chlorpromazine Colorimetric Fectrophotometric; stability olumetric, amperometric Chromatographic; spectrophotometric Cholecalciferol Cholesterol and cholesteryl esters Chromatographic, column Chromatographic, thin layer Chrysarobin Chromatographic; spectrophotometric Coamide Colorimetric, ion-pair Coca leaf Review, pharmacopeia1 methods Cola Chromatographic, column; thin layer Colistin Automatic analysis Colorimetric Colorimetric, ion-pair Cordiamin Cyclamates Chromatographic; volumetric Review Cyclazocine Chromatographic, gas; thin layer {1614B) Chromatographic; colorimetric Cyclizine (1284) Chromatographic, gas; thin layer (2303) Cyclobarbital Chromatographic, g y ($303) Chromatographic, thm layer (1809. 2303) Volumetric, amperometric Cyclopyrin Chromatographic, thin layer Cytochrome Stability; oxidative degradation Decamethonium iodide Chromatographic, paper; thin layer Deco uinate Chromatographic; fluorometric Colorimetric Dehy%ocholic acid Dehydromatricaric ester Chromatogra hic, paper Differential tierma1 analysis Deoxycholic acid Automatic analysis; spectrophotometric Desipramine Detropine Chromatographic; colorimetric Dexamphetamine Identification Chromatographic, thin layer; fluorometric Dextromethorphan Diacetyldihydroxydiphenylisatin Colorimetric Diatrizoic acid Chromatographic, thin layer Dibazole Chromatographic, thin layer Microcrystallographic S ectrophotometric, ultraviolet olumetric, acid-base, nonaqueous Dicyclomine Microcrystallographic Diethazine S ectrophotometric; stability Qolumetric, acid-base, nonaqueous Diethylphthalate Chromatographic, thin layer Digamnocaine X-ray diffraction Digitoxin Chromatographic; colorimetric Diisopromine Microcrystallographic Dimedrol Chromatographic, thin layer Volumetric, acid-base, nonaqueous N,N-Dimethyltryptamine Fluorometric Dimethyluracil Complex formation Diodone Chromatographic; spectrophotometric Volumetric, ox.-red. X-ray diffraction Diothane Diphedan Chromatogra hic, gas Diphenylhydantoin Differential tlermal analysis Diphenylhydramine Chromatographic, thin layer Chelatometric Colorimetric Microcrystallographic Colorimetric Diprofen Volumetric, ox.-red. Dispasmol s ot tests Diuretin romatographic, thin layer Volumetric, acid-base, nonaqueous n-Dodecylamine Volumetric, acid-base, nonaqueous Dospan Chromatographic, thin layer Effortil Chromatographic, thin layer Ethisterone Chromatographic, thin layer Ethoxybenzamide Spectrophotometric, ultraviolet B Analysis of pharmaceuticals in biological media.
Compound or Class Chloramphenicol
vp
CR
(Continued on next page)
ANALYTICAL CHEMISTRY, VOL. 43,
NO. 5,
APRIL 1971
237 R
Table IX.
Formulations, Mixtures a n d G e n e r a l Methods (Continued)
Compound or Class Ethylene chlorohydrin Ethylenediamine Ethylene oxide Ethyl-7-flavonoxyacetate Ethyl linoleate Fennel Fraxinus plants Furacain Furazolidone Galipyrin Gallamine Glucose Glutethimide Halazuchrome B Halo thane Hexahydroadiphene Hexamethylene-tetramine Hexermin P Hexylresorcinol Homopantothenic acid Hydrochlorothiazide Hydrocinnamic acid Hydroquinone p-Hydroxybenzoates
Method or Subject Chromatographic, column; gas Chromatographic, thin layer Chromatographic, gas Chromatographic; spectrophotometric Chromatographic, gas Chromatographic, thin layer Chromatographic,, paper; thin layer Spectrophotometric; stability Chromatographic; densitometric Chromatographic, thin layer Chromatographic,, paper; thin layer Automatic analysis; colorimetric Chromatographic, thin layer Chromatographic; spectrophotometric Impurities in; chromatographic, gas Chromatographic, thin layer Colorimetric Chromatographic, thin layer Stability to infrared radiation Chromatographic; colorimetric Volumetric, amperometric Complex formation Volumetric, ox.-red. Chromatographic, thin layer Partition coefficients 17~-Hydroxy-7cu-17cu-dimethyl- Colorimetric 0-homo-A-norestrane3,6-dione Imipramine Automatic analysis; spectrophotometric India clove Chromatographic thin layer Indopan Identification 0-Iodohippuran 1311-labelled; chromatographic; radiometric Iodohippuric acid Chromatographic; spectrophotometric Isobutyl-4-aminobenzoate Microcrystallographic Isoniazid Chromatographic, paper Volumetric, conductometric Isonicotinic acid Chromatographic; colorimetric Isoprenaline Colorimetric Volumetric, conductometric Isopropylantipyrine Chromatographic, thin layer Colorimetric Spectrophotometric Isoptin Microcrystallographic Isopyrine Volumetric, ox.-red. Isothipendy Spectrophotometric; stability Kimopsin Chromatographic, thin layer Lachesine Stability Lantrol Chromatographic, thin layer Levorphanol Identification, review Lidocaine Volumetric, acid-base, nonaqueous Linden flowers Chromatographic, thin layer Liver preparations Electrophoretic Marine liver oils Arsenic in; neutron activation analysis %IDS Chromatographic, thin layer Measle vaccines Nitrogen content; Kjeldahl Meclizine S ectrophotometric, ultraviolet Medinal Tfolumetric, acid-base, nonaqueous Menadione Complex formation Menthol Chromatographic, thin layer Meprobamate Automatic analysis; colorimetric Mercazole Chromatographic, thin layer RIerkazolil Volumetric, ox.-red. Mesocaine Spect ropho tome t ri e, ultraviolet Rlestranol Chromatographic; colorimetric Metaclopramide Xlicrocrystallographic Methapyrilene Automatic analysis Chromatographic, gas Chromatographic; spectrophotometric Methionine Automatic analysis; colorimetric Volumetric, microcolorimetric Methocarbamol Spectrophotometric, ultraviolet Methylamphetamine Chromatographic, thin layer Identification Methylcinnamate Complex formation 11icrocrystallographic p-Met hyldiphenhydramine Spectrophotometric, ultraviolet Methylphenidate Chromatographic, thin layer Rlethylpropamine Chromatographic, gas Volumetric, ox.-red. 1Iethylthiouracil Meza t on Identification Mint Chromatographic, thin layer Analysis of pharmaceuticals in biological media.
Reference
(610; 2256)
(1672) (740)
(1526)
(1090) (968B) (1373B) (949) (2245) (1090)
(1496) (1398) !??&6) (2334) (Continued on next
238R
ANALYTICAL CHEMISTRY, VOL. 43, NO, 5, APRIL 1971
~~
Compound or Class Monocaine Naphazoline Neomycin Neophyllin Neostigmine Neuzyn Nicodine Nifuroxime Nitrobenzene Nitrogen Nitrowarfarin Noradrenaline Norcyclazocine Novalgin Novamin Parabens
Paramethazone Parpokan Pecazine Pentetrazole Pentobarbital Peppermint water Perphenazine Phenacaine Phenacetin
~
~
Table IX. Formulations, Mixtures, and General Methods (Confinued) Method or Subject Reference X-ray diffraction (1000) Chromatographic, paper (1637) Chromatographic, column (312) Chromatographic, thin layer (1428) Chromatographic, thin layer (2089) Chromatographic, thin layer (1428) Colorimetric, ion-pair (1111) Chromatographic; densitometric (216) Spectrophotometric, ultraviolet (1090) Kjeldahl (1528) Volumetric, amperometric (1232) Volumetric, conductometric (1150) Chromatographic, .gas; thin layer (15148) Identification, review (1676) Volumetric, acid-base (2160) Chromatographic, thin layer (1428) Chromatographic (1314) Chromatographic, thin layer ( 1780, 1781) (1314) Fluorometric Partition coefficients (1524) Automatic analysis; colorimetric (1974) Spot tests (1501) Chromatographic, thin layer (1809) Volumetric, acid-base, nonaqueous Chromatographic, gas; extractive Chromatographic, thin layer (430B) Volumetric, acid-base, nonaqueous (J7) Chromatographic, gas (934) Spectrophotometric; stability (8711 X-ray diffraction (2000) Automatic analysis (.@OB,885) Chromatographic, gas (435, 510, 1546, 2303) (5531 Chromatographic, paper Chromatographic, thin layer (95, 346, 508, 101gB, 1260, 1339, 1811, 2106,2303) Complex formation (949) Densitometric (608) Differential thermal analysis (744) Extractive ; gravimetric Identification, review Spectrophotometric, ultraviolet (510, 1793-1796) Thermal analysis (885, 886) Volumetric, ox.-red. (462) Chromatographic; spectrophotometric (3691 Chromatographic, thin layer (1496) Chromatographic; spectrophotometric (628) Complex formation (949) Complex formation (949) Automatic analysis (1546) Spectrophotometric, ultraviolet (1095) Chromatographic, thin layer (1496) Identification (lSY3B) Chromatographic, gas (513) Chromatographic, thin layer (96, 362, ,$SOB, 508, 1327, 1339, 1781, 1809, 1811) Colorimetric (2046, 2058) Densitometric (608) Differential thermal analysis (7441 Electrodialysis (574) Electrophoretic, paper (931 Extractive; gravimetric (113) Microcrystallographic (1641) Spectrophotometric (2333) Spectrophotometric, ultraviolet (540) Volumetric, acid-base, nonaqueous (2327) Volumetric, precipitation (2345) Extractive; gravimetric (113) Chromatographic, thin layer (1496) Chromatographic, thin layer (1552, 1553, 1808, 1809, 1916) Identification, review (1675) Chromatographic, thin layer; fluorometric (11429 Automatic analysis ; colorimetric (510) Neutron activation analysis, of Ag complex (235) G r avimet r ic (340) Volumetric, amperometric (1232) Chromatographic, thin layer (25,941 Volumetric, amperometric (1232) Chromatographic, paper (8)
((8%
[KL)
Phenatine Phendimetrazine Phenethyl alcohol Phenethylamine Phenethyl ammonium ion Phenformin Pheniodol Phenmetrazine Phenobarbital
Phenolphthalein Phentermine Phenylbutazone Phenylephrine Phenylpropanolamine Phenylsalicylate Phthalylsulfathiazole Plivadon Plurisulfane comprimate Poly(oxyethy1ene) sorbitans; esters E
Chromatographic; spectrophotometric Analysis of pharmaceuticals in biological media.
(3200)
(Continued on next page)
ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
239 R
Table IX. Formulations, Mixtures, and General Methods (Continued) Method or Subject Chromatographic Spectrophotometric Stability Prednisolone Chromatographic; colorimetric Primacaine X-ray diffraction Primperan Chromatographic, thin layer Procaine Automatic analysis; colorimetric Chromatographic, paper Chromatographic, thin layer S ectrophotometric, ultraviolet dlumetric, acid-base, nonaqueous Volumetric; complexometric (88ij X-ray diffraction (2000) Procaine penicillin Automatic analysis; colorimetric (1666) Promazine Volumetric, complexometric f881) ’ Promedol Volumetric, acid-base, nonaqueous Promethazine Chromatographic; spectro hotometric Spectrophotometric; stabiEty Propamine Chromatographic, gas Propanidid Enzymatic; spectrophotometric, ultraviolet Propoxyphene Automatic analysis; colorimetric Chromatographic; colorimetric Colorimetric Identification, review Propylhexedrine Chromatographic, thin layer Protamine Photometric, light-scattering Protriptiline Chromatographic, thin layer Psilocybin Fluorometric Pyrilamine Chromatographic,. partition Spectrophotometric, ultraviolet Redwater tree Chromatographic, thin layer Remeflin Chromatographic, thin layer Resorcinol Volumetric, amperometric Rosemary Chromatographic, thin layer Rutin Chromatographic, thin layer Spectrophotometric, ultraviolet Stability Chromatographic, gas Sacerno Salicylamide Chromatographic, thin layer Spectrophotometric, ultraviolet Salicylic acid Chromatographic, partition column Chromatographic, thin layer Spectrophotometric, internal reflectance Spectrophotometric, ultraviolet Salimed Chromatographic, thin layer Sarcosine anhydride Complex formation Septonex Chromatographic, thin layer Sodium barbiturate Chromatographic, paper Electrophoretic,. paper Sodium benzoate Chromatographic, thin layer Volumetric, acid-base, nonaqueous Sodium caffeine benzoate Volumetric, acid-base, nonaqueous Sodium cholate Chromatographic, ion exchange Sodium cyclamate Chromatographic, ion exchange Sodium merthiolate Chromatographic, thin layer Sodium salicylate Chromatographic, paper Electrophoretic, paper Microcrystallographic Sodium sulfacetamide Volumetric, acid-base, nonaqueous Spot tests Spasman Colorimetric Spasmolitine Chromatographic; mass spectrometric Spermaceti Chromatographic, column Spikenard oil X-ray diffraction Stovaine Chromatographic, paper; thin layer Succinylcholine chloride Chromatographic; spectrophotometric Sulfacetamide Chromatographic, column Sulf amethoxypyridazine Sulfanilamide Chromatographic, gas Chromatographic; spectrophotometric Sulfathiazole Volumetric, amperometric Chromatographic, thin layer Sulpyrin Volumetric, acid-base Sulthiame Colorimetric; ion-pair Suprastin Chromatographic, thin layer Surgical spirits Fractional distillation Tar Colorimetric Tetracaine X-ray diffraction Automatic analysis; colorimetric Tetracycline Review Complex formation Tetramethyl succinamide
Compound or Class Pralidoxime
B
Analysis of pharmaceuticals in biological media.
(Continued on next page)
240R
ANALYTICAL CHEMISTRY, VOL. 43,
NO. 5, APRIL 1971
Table IX. Formulations, Mixtures, and General Methods (Continued) Method or Subject Electrophoretic, paper Volumetric, complexometric Chromatographic, thin layer Volumetric amperometric Colorimetri'c Microcrystallographic Volumetric, ox;-red. Chromatographic, thin layer TMPDS Suectrouhotometric. ultraviolet Tolazoline Tolbutamide C'hrom&ographic, thin layer Triamcinolone acetonide Chromatographic; fluorometric Triiotrast Spot tests Trimethylene-bis [ 4Spectrophotometric, ultraviolet (hydroxyiminomethy1)py~idinium] dibromide(TMB-4) Trinitrin Automatic analysis; colorimetric Triolein Chromatographic, column Triperidol Microcrystallographic Unicaine X-ray diffraction Vitamin PP Chromatographic, thin layer Water Chromatographic, gas Xanthydrol Chromatographic; colorimetric
Compound or Class Thebaol Thonzylamine Thyme Thymol Tifen
LITERATURE CITED
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(200) Blazek, J., Famnatsiya (Moscow), 18 (5), 76-80 (1969); Chem. Abstr., 72, 24656 (1970). (201) Blazek, J., Pinkasova, M., Cesk. Farm., 17, 181-189 (1968); Chem. Abstr., 69, 46123 (1968). (202) Zbid., 18, 314-323 (1969); Chem. Abstr., 72, 47402 (1970). (203) Blazek, J., Spinkova, V., ibid., 16, 201 (1967); Anal. Abstr., 15, 4879 (1968).
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(314) Cavatorta L., Romaniello, E., Allievi, R., B o k Chim. Farm., 107, 721725 (1968); Chem. Abstr., 70, 80889 (1969’I. G., Quercia, V., Calo, ‘36; Chem. Abstr., 70, Giocoli, G., Ann. 1st. Super. Sanita, . 4 (Pt. 1-2), 101-102 (1968): Chem. Abstr.., 69.. 697042 (1968j: (317) Cavina, G., Moretti, G., Sardi de Valverde, J., ibid., pp 75-89; Chem. Abstr., 69, 69703 (1968). (318) Cavina, G., Moretti, G., Siniscalchi, P., Int. Symp. Chromatogr. Electrophor., Proc. 6th, 21, 447-463 (1968). (319) Cerdas, J., Carlier, A., Puisieux, F., Le Hir, A., Ann. Pharm. Fr., 25, 553 (1967); Anal. Abstr., 15, 6922 (1968). (320) Cerdas, J., Carlier, A., Puisieux, F., Le Hir, A., ibid., 26 (3), 239-244 (1968); Chem. Abstr., 69, 46113 (1968). (321) CerB, L., Barolo, P., Ann. Chim. (Rome), 57, 1288 (1967); Anal. Abstr., 16, 931 (1969). (322) CerB, L., Bongiovann, G., Mondino, A,, ibid., 58, 1163-1172; Chem. Abstr., 70, 40656 (1969). (323) Cerri, O., Boll. Chim. Farm., 108, 217-22 (1969); Chem. Abstr., 71, 53637 (1969). (324) Chafetz, L., Boudjouk, M. G., Tsilifonis, D. C., Hom, F. S., J . Pharm. Sci., 57, 1000-1003 (1968). (325) Chafetz, L., Daly, R. E., ibid., pp 1977-1979. (326) Chafetz, L., Kay, A. I., Schriftman, H., J . Chromatogr.,35, 567 (1968). (327) Chaigneau, M., Chastagnier, M., Ann. Pharm. Fr., 25 (6), 463466 (1967); Anal. Abstr., 15, 5593 (1968). (328) Chakravarti, R. N., J . Inst. Chem. (India), 40 (Pt. 2), 42-48 (1968); Chem. Abstr., 69, 54256f (1968). (329) Ibid., (Pt. 3), 85-101; Chem. Abstr., 68, 77549 (1968). (330) Chanal, J. L., Marignan, R., Coste, J. M., Trav. SOC.Pharm. Montpellier, 29, 53-60 (1969); Chem. Abstr., 71, 105167 (1969). (331) Ibid., pp 61-65; Chem. Abstr., 71, 105168 (1969). (332) Chandra, S., Yadava, K. L., Microchem. J., 13, 586-591 (1968); Anal. Abstr., 18,2484 (1970). (333) Chandra, U., Tayal, J. N., Nand, P., Fresenius’ Z. Anal. Chem., 238, 457-459 (1968); Chem. Abstr., 69, 99436 (1968). (334) Chapman, J., Hill, It., Muir, J., Suckling, C. W., Viney, D. J., J. Pharm. Pharmacol., 19, 231 (1967); Anal. Abstr.. 15,4232 (1968). (335) Char;-Bitron, A:, Bino, T., Ind. Chim. Belge, 32, 93 (1967); Anal. Abstr., 15.7114 (1968). (336) Charranso, G., Desfosses, B., J . Eur. Steroides, 2, 423441 (1967); Chem. Abstr., 70, 11874j (1969). (337) Chatten, L. G., Ed., “Pharmaceutical Chemistry, Vol. 2; Instrumental Techniques,” Dekker New York, 1969, 773 pp. (338) Chatten, L. G., Barry, P. J., Can. J . Pharm. Sci., 3, (2), 40-45 (1968); Chem. Abstr., 70, 22934 (1969). (339) Chausovskii, S. S., Farmatsiya (M05CW), 17 (2), 4 8 4 9 (1968); Chem. Abstr.. 69.21957 (1968). (340) Chedakowski‘ Am M., Mosiniak, T., Acta Pol. k’harm., 24, 511-513 (1967); Anal. Abstr., 15, 4979 (1968). (341) Chekryshkina, L. A,, Nauch. Tr. Asair. Ordinatorov. 1-i Mosk. Med. Inst., 1967,160-162; Ckem. Abstr., 70,50492c (1969). ’
(342) Chekryshkina, L. A,, Shemyakin, F. M., Farm. Zh. (Kiev), 24 (3), 50-52 (1969); Chem. Abstr., 71, 53613 (1969). (343) Chemrisska a A. A:, Tubina, I. S., Egorova, T. Khzm.-Farm. Zh., 3 (2), 29-32 (1969); Chem. Abstr., 71, 6582d (1969). (344) Chemerisskaya, A. A., Tubina, I. S., Egorova, T. N., Galstukhov, V. P., ibid.. 1 (8).45-47 (1967): Chem. Abstr.. 69. 24377’?1968).
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246R
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(561) Zbid., 34 (193), 15596-7 (Oct. 8, 1969). (862) Fellig, J., Westheimer, J., J . Agr. Food Chem., 16,738 (1968). (563) Fenner, H., Fresenius’ 2. Anal. Chem., 249, 124-127 (1970); Chem. Abstr., 72,93357 (1970). (564) Fernandes, A. A., Noceda, T. V., J . Pharm. Sci., 58,740-744 (1969). (565) Fernandez, J., Ek, L., Leeper, L. C., Automat. Anal. Chem., Technicon Symp., Srd, 1967, 1, 471-476. (566) Feroci, M., Orzalesi, G., Selleri, R., Boll. Chim. Farm., 108,313-323 (1969); Chem. Abstr., 71, 1052422 (1969). (567) Ferrando, R., Renard, A., Bull. SOC. Chim. Biol.. 50. 1855 (1968): , , Anal. Abstr., 18, 1279 (1970). (568) Ferrari, H., Therm. Anal., Proc. Znt. Conf., 2nd, 1968, 1, 41-64; Chem. Abstr., 72, 357373 (1970). (569) Ferreira, L. G., Nobrega, P., Nobrega, M. A. F., Rev. Brasil. Farm., 48, 26.5-279 (1967); Chem. Abstr., 69, 5262 11968). (57O)-Ferren, W. P., Shane, N . A., J . Ass. OBc. Anal. Chem., 51, 573 (1968). (571) Fickentscher, K., Deut. Apoth.-Ztg., 108, 154.5-1546 (1968); Chem. Abstr., 70, 31722 (1969). (572) Fidecka, H., Ann. Univ. Mariae Curie-Sklodowska, Sect. DD, 1966, 21, 139-143 (1967); Chem. Abstr., 69, 30167 (1968). (573) Filippos’yants, T. T., Poadnyakova, Z. E., Sandomirskaya, G. A., Khim.Farm. Zh., 2 (4), 56-58 (1968); Chem. Abstr. 69, 38723a (1968). (574) Finholt, P., Pedersen, J. H., Med. Norsk. Farm. Selsk., 30, 115 (1968); Anal. Abstr., 18, 1439 (1970). (+576)Finkel, J. M., Anal. Biochem., 21, 362-371 (1967). (576) Finkel, J. M., Knapp, K. T., ibid., 25,465 (1968). (577) Fiori, A., Marigo, M., J . Chromatogr., 31, 171 (1967). (578) Firth, R. A., Hill, H. A. O., Pratt, J. M., Thorp, R. G., Anal. Biochem., 23,429 (1968). (579) Fischer, A., Chromatographia, 1, 481-482 (1968); Anal. Abstr., 18, 2551 (1970). (580) Fischer, G., Vegh, A., Acta Pharm. Hung., 38, 1-5 (1968); Chem. Abstr., 68, 119274m (1968). (581) Fischer, R., Midula, G., Arzneim.Forsch., 19, 2025-2026 (1969); Chem. Abstr., 72, 59131 (1970). (582) Fish, F., Kirk, W. R., J . Chromatogr., 36, 383 (1968). (583) Fishbein, L., ibid., 30, 245 (1967). (584) Flsnn, B. C., J . Pharm. Sci., 58, 122-124 (1969). (585) Fletcher, G., Davies, D. J. G., J . Pharm. Pharmacol., 20, (Suppl.), 1085 (1968); Anal. Abstr., 18, 2724 (1970). (586) Flom, M. S., Doskotch, R. W., Beal, J. L., J . Pharm. Sci., 56, 1515-1517 (1967). (587) Floret, G., Massa, V., Chromatogr., Electrophor., Symp. Int., 4th, 1966 138-144 (1968); Chem. Abstr., 72, 47406 (1970). (588) Floret, G., Massa, V., Trav. SOC. Pharm. Montpellier, 28, 129-137 (1968); Chem. Abstr., 70, 31731p (1969). (589) Fogg, A. G., Sausins, P. J., Smithson, J. R., Anal. Chim. Acta, 49, 342345 (1970). (590) Fokkens, J., Burman, E., Pharm. Weekbl., 104 (9), 177-183 (1969); Chem. Abstr., 70, 90714 (1969). (591) Fontanelli, L., Silvestri, S., Farmaco, Ed. Prat., 24, 719-724 (1969); Chem. Abstr., 72,47393g (1970). (592) Fooks,. J. R., Mattok, G. L., J . Pharm. Sa.,58, 1357-1359 (1969). ~
(5931 Forman. B. J.. Gradv. L. T., ibid..
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(623) Fuwa, T., Suzuki, M., Kido, T., Okamura, F., Yakuzaigaku, 27, 345-347 (1967); Chem. Abstr., 69, 109860 (1968). (624) Gaidano, G., M o h o , G., Angeli, A., Perotti, L., Boccuzzi, G., Boll. SOC. Ztal. Biol. Sper., 64, 1494 (1968); Anal. Abstr., 16, 2637 (1969). (625) Gaidano G., M o h o , G. Perotti, L., Matta, b., Boccuzzi, G., ibid., pp 1494-1497; Chem. Abstr., 70, 90789 f1969). (626jvGainer, F. E., Arnett, W. A., J . Pharm. Sci., 58, 1548-1550 (1969). (627) Gal’pern, G. M., Andrianov, V. F., Levit. N. P.. Shcherbik. L. K.. Lisnvanskii, I. M.,’ Khim.-Farm. Zh., 1 “(S), 48-50 (1967); Chem. Abstr., 69, 61568n (1968). (628) Gandel, V. G., Nekrasov, V. I., Farmatsiya (Moscow), 17, 27-30 (1968); Chem. Abstr., 68, 98690 (1968). (629) Ganguly, S. K., Ghosh, B. P., Bull. Znst. Post Grad. Med. Educ. Res., 10, 27-32 (1968); Chem. Abstr., 70, 14467q (1969 ). \ _ _ _ _
(630) Ganis, F. M., Lipid Chromatogr. Anal., 2, 1-55 (1969). (631) Garber, C., Aseem, E. M., Pinol, L. hI., SAFYBI, 8 (25), 33-43 (1968); Chem. Abstr., 70, 22976 (1969). (632) Garber, C., Dobrecky, J., Rev. Asoc. Bioquim. Argent., 33 (178-179), 180184 (1968); Chem. Abstr., 72, 35816 (1970) ,--.-,.
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(684) Gorbach. G.. Henke. J.. Hekal. I.. ’ Mikrochim. Acta: 1968, 8861893; Anal: Abstr., 17, 3088 (1969). (685) Gore, A. Y., Naik, K. B., Kildsig, D. O., Peck, G. E., Smolen, V. F., Banker, G. S..J . Pharm. Sci., 57, 18501854 (1968). ’ (686) Gore. T. S.. Inemdar. P. K.. Mikro‘ chim. A’cta, 1968, 883-885;’ Chem. Abstr., 69, 56877 (1968). (687) Gorog, S., ActaChim. (Budapest),61, (4), 341-347 (1969); Chem. Abstr., 71, 105247 (1969). (688) Gorog, S., J . Pharm. Pharmacol., 21 (Suppl.), 46-48 (1969); Chem. Abstr., 72. 35819n (1970). (689) Gorog, S., J . Pharm. Sci., 57, 17371741 (1968). (690) Gorog, S., Magy. Kem. Foly., 74, 447-450 (1968); Chem. Abstr., 70, 14446g (1969). (691) Ibid., 75, 509-513 (1969); Chem. Abstr., 72, 6261 (1970). (692) Gorog, S., Steroids, 11, 93-95 I
,
(1968). \----,.
(693) Goryacheva, N. S., Prikhodkina, L. N., Farmatsiya (Moscow), 17 (3), 69-72 (1968): Chem. Abstr., 69, 61575n (1968). (694) Goto, E., Furukawa, T., Goto, S., Yakuzaigaku, 27 (4), 311-313 (1967). (695) Gotovtseva, V. A., Gusakova, E. G., Korovkina, A. S., Lab. Delo, 1969 (2), 101-102; Anal. Abstr., 18, 3383 (1970). (696) Gouezo, F., Raman, J. P., Cristau, B., Ann. Pharm. Fr., 26 (4), 301-310 (1968); Chem. Abstr., 6 9 , 5 4 3 1 1 ~(1968). (697) Grab, F. L., Reinstein, J. A., J. Pharm. Sci., 57, 1703 (1968). (698) Graber, X.1. B., Domsky, I. I., Ginn, &I. E., J . Amer. 0 2 1 Chem. SOC.,46 (lo), 529-531 (1969). (699) Grabowicz, W., Acta Pol. Pharm., 25, 353-354 (1968); Chem. Abstr., 70, 40664 (1969). (700) Grabowicz, W., Chem. Anal. (Warsaw), 13, 1273-1277 (1968); Chem. Abstr., 71, 24768 (1969). (701) Grabowska, I., Acta Polon. Pharm., 25, 423 (1968); Anal. Abstr., 17, 1700 (1969). (702) Grabowska, I., Acta Pol. Pharm., 26, 543-547 (1969); Chem. Abstr., 72, 93360 (1970). (703) Grabowska, I., Farm. Polska., 24, 565 (1968); Anal. Abstr., 17, 3760 (1969). (704) Gracian, J., Martel, J., Grasas Aceztes, 19 (4), 135 (1968); Chem. Abstr.. 70. 14449k (1969). . , (703) Gianik, E. M., Chemerisskaya, A. A., Khim.-Farm. Zh., 2 (lo), 4 1 4 4 (1968): Chem. Abstr., 70,31729~(1969). (706) Idid., 3 (2), 32-36 .(1969); Chem. Abstr., 71, 65771 (1969). (707) Grant, D. J. W., Patel, J. C., Anal. Biochem., 28, 139-149 (1969); Chem. Abstr., 70, 90794 (1969). (708) Grecu, I., Barbu, S., Ann. Pharm. Fr., 26, 405408 (1968); Chem. Abstr., 69, 69709 (1968). (709) Ibid., pp 493495; Chem. Abstr., 72. 24698 (1970). (710j Grecu, ’ I., ’Barbu, S., Farmucia (Bucharest), 16, 199-204 (1968); Chem. Abstr., 69, 12950x (1968). (711) Ibid., 327-330; Chem. Abstr., 69, 46122 (1968). (712) Grecu, I., Curea, E., Farmaco, Ed. Prat., 23, 603-612 (1968); Chem. Abstr.. 70. 31726 (1969). . , (713) Giecu, I., Curea, E., Reo. Roum. Chim., 13, 781 (1968); Anal. Abstr., 17, 3004 (1969). (714) Gregorowicz, Z., Piwowarska, B., Rnhl. -... F.. Kania. K.. Fresenius’ 2. Anal. Chem., 237, 347-351 (1968); Chem. Abstr., 69, 32876 (1969). I
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7 - -
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ANALYTICAL CHEMISTRY, VOL. 43, NO. 5, APRIL 1971
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~I
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