BRIEFS
Articles
Adaptation of a Thermospray Liquid Chromatography/Mass Spectrometry Interface for Use with Alkaline Anion Exchange Liquid Chromatography of Carbohydrates 248
Automated Selection of Library Subsets for Infrared Spectral Searching 226
An interface is described for coupling alkaline anion ex change HPLC with thermospray MS. Sugars are used as model compounds to evaluate system performance in both the isocratic and gradient elution modes. Mass spectra ob tained on line are compared with those obtained by the direct injection method. Richard C. Simpson* and Catherine C. Fenselau, Department of Chemistry and Biochemistry, University of Maryland, Baltimore County, Baltimore, MD 21228, Mark R. Hardy, R. Reid Townsend, and Yuan C. Lee, Department of Biology, Johns Hopkins University, Baltimore, MD 21218, and Robert J. Cotter, Depart ment of Pharmacology, Johns Hopkins University, Baltimore, MD 21205
Principal components analysis is used to select an appropri ate subset of an FT-IR spectral library for subsequent Eu clidean distance searching. Based on the relationships be tween library spectra and the computed principal compo nents of the library, a series of ordered lists are created that help to pinpoint similar spectra. Joanne M. Bjerga and Gary W. Small*, Department of Chemis try, The University of Iowa, Iowa City, IA 52242 Accuracy of Peak Deconvolution Algorithms within Chromatographic Integrators
234
Determination of Regulatory Organic Compounds in Radioactive Waste Samples. Semivolatile Organics in Aqueous Liquids 253
Significant chromatographic peak deconvolution parame ters (minimizing inaccuracies for the tangent skim and per pendicular drop deconvolution methods) are compared with the parameters used by commercial integrators. Andrew N. Papas*, U.S. Food & Drug Administration, Winchester Engineering and Analytical Center, Winchester, MA 01890 and Terrence P. Tougas, Chemistry Department, University of Lowell, University Avenue, Lowell, MA 01854
Regulatory semivolatile organic compounds are readily ex tracted from small volumes of aqueous, highly radioactive liquids and quantitated in a conventional GC/MS labora tory. Bruce A. Tomkins*, John E. Caton, Jr., G. Scott Fleming, Manuel E. Garcia, Sara H. Harmon, Robert L. Schenley, Cheryl A. Treese, and Wayne H. Griest, Organic Chemistry Sec tion, Analytical Chemistry Division, Oak Ridge National Laborato ry, Oak Ridge, TN 37831-6120
Measurement of Vanadium Impurity in Oxygen-Implanted Silicon by Isotope Dilution and Resonance Ionization Mass Spectrometry 240 Trace analysis is performed on surface layers that are chemi cally removed from a semiconductor material and weigh < 1 mg. Picogram levels of vanadium are detected. Santos Mayo, Semiconductor Electronics Division, National Insti tute of Standards and Technology, Gaithersburg, MD 20899 and John D. Fassett*, Howard M. Kingston, and Richard J. Walker, Inorganic Analytical Research Division, National Institute of Stan dards and Technology, Gaithersburg, MD 20899
Cross-Linked Redox Gels Containing Glucose Oxidase for Amperomotric Biosensor Applications 258 Two materials, based on a cross-linkable poly(vinylpyridine) complex of [Os(bpy)2Cl] +/2+ that communicates elec trically with flavin adenine dinucleotide redox centers of enzymes such as glucose oxidase, are described for use in amperometric biosensors. The glucose response time of the resulting electrode is < 10 s. Brian A. Gregg and Adam Heller*, Department of Chemical Engineering, University of Texas at Austin, Austin, TX 78712
Application of Countercurrent Chromatography/Thermospray Mass Spectrometry for the Identification of Bioactive Lignans from Plant Natural Products 244
Flow System for Starch Determination Based on Consecutive Enzyme Steps and Amperometric Detection at a Chemically Modified Electrode 263 Starch is totally hydrolyzed to glucose by using immobilized α-amylase and amyloglucosidase. Coimmobilized mutarotase and glucose oxidase oxidize glucose to hydrogen perox ide, which is amperometrically detected. Calibration curves are linear between 10 μΜ and 0.6 mM. Sample throughput is 15 h~'. J. Emnéus and L. Gorton*, Department of Analytical Chemistry, University of Lund, P.O. Box 124, S-221 00 Lund, Sweden
The capability of thermospray CCC/MS is demonstrated in identifying and validating the bioactive and structurally known lignans from a crude extract of Schisandra rubriflora Rhed et Wils, a traditional Chinese herbal medicine for the treatment of hepatitis. Yue Wei Lee*, Robert D. Voyksner, Terry W. Pack, and C. Edgar Cook, Research Triangle Institute, P.O. Box 12194, Re search Triangle Park, NC 27709, Q. C. Fang, Institute of Materia Medica, Chinese Academy of Medical Sciences, Beijing, China, and Yoichiro Ito, Laboratory of Technical Development, National Heart, Lung, and Blood Institute, Bethesda, MD 20892
* Corresponding author
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112 A · ANALYTICAL CHEMISTRY, VOL. 62, NO. 3, FEBRUARY 1, 1990
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BRIEFS Simulation of Two-Electron Homogeneous Electrocatalysis tor Steady-State Voltammetry at Hemispherical Microelectrodes 268 Simulations of two-electron homogeneous electrocatalysis for hemispherical microelectrodes show that as electrode radii decrease, larger catalytic rates are needed for significant current amplification. Chang Ling Miaw, James F. Rusling*, and Azita Owlia, Department of Chemistry (U-60), University of Connecticut, Storrs, CT 06269-3060 Determination of Copper at Electrodes Modified with Ligands of Varying Coordination Strength: A Preamble to Speciation Studies 274 To ascertain the use of chemically modified electrodes in speciation studies, electrodes modified with seven different ligands whose formation constants for copper vary over a broad range are used to determine copper in solution. Seong K. Cha and Hector D. Abrufia*, Department of Chemistry, Baker Laboratory, Cornell University, Ithaca, NY 14853-1301 Determination of Linkage Position and Identification of the Reducing End in Linear Oligosaccharides by Negative Ion Fast Atom Bombardment Mass Spectrometry 279 The reducing end and monosaccharide sequences are identified, and the 1-4, 1-6, 1-3, and 1-2 linkage positions are discriminated by analysis of the negative metastable ions produced in FAB-MS linked scans. Domenico Garozzo, Mario Giuffrida, and Giuseppe Impallomeni, Istituto per la Chimica e la Tecnologia dei Materiali Polimerici, Consiglio Nazionale delle Ricerche, Viale A. Doria 6, 95125 Catania, Italy and Alberto Ballistreri and Giorgio Montaudo*, Dipartimento di Scienze Chimiche, Université di Catania, Viale A. Doria 6,95125 Catania, Italy
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Nitric Oxide Chemical Ionization Mass Spectrometry of LongChain Unsaturated Alcohols, Acetates, and Aldehydes 287 CI-NO+-MS is used to determine double bond location in long-chain monounsaturated alcohols, acetates, and aldehydes, mostly through the formation of an acylium diagnostic ion. An extension of the method for assigning the external double bond in di- or tri-ethylenic compounds is described. Christian Malosse and Jacques Einhorn*, INRA-CNRS, Laboratoire des Médiateurs Chimiques, Magny-les-Hameaux, 78470 StRémy-les-Chevreuse, France Amperometric Monitoring of Ozone in Gaseous Media by Gold Electrodes Supported on Ion Exchange Membranes (Solid Polymer Electrolyes) 293 An in situ amperometric sensor is described that permits a limit of detection of ÎO - 8 M (0.5 μ% L" 1 , 2.24 Χ 10~7 atm) with a response time of 0.5 s. Gilberto Schiavon* and Gianni Zotti, CNR-IPELP, corso Stati Uniti 4, 1-35100 Padova, Italy, Gino Bontempelli*, Institute of Chemistry, University of Udine, viale Ungheria 43,1-33100 Udine, Italy, and Giuseppe Farnia and Giancarlo Sandonâ, Department of Physical Chemistry, University of Padova, via Loredan 2,1-35131 Padova, Italy
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Comparison of Photoacoustic Spectroscopy, Conventional Absorption Spectroscopy, and Potentiometry as Probes of Lanthanide Speciation 298
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Photoacoustic spectroscopy provides the same information about the number and strength of metal-ligand complexes as conventional absorption spectroscopy or potentiometry at metal concentrations where the latter techniques are insensitive. Richard A. Torres*, Cynthia E. A. Palmer, Patricia A. Baisden, Richard E. Russo, and Robert J. Silva, Lawrence Livermore National Laboratory, P.O. Box 808, L-234, Livermore, CA 94551
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Kinetic studies of the Schiff base formation reaction between aromatic aldehydes and o-dianisidine provide evidence of a three-path mechanism. Two paths are catalyzed by acetic acid and the other by stannic chloride. Analytical implications of the kinetic studies are discussed. Mayda Lopez-Nieves, Peter D. Wentzell, and S. R. Crouch*, Department of Chemistry, Michigan State University, East Lansing, MI 48824
Correspondence Comparison of Diffuse Reflectance and Diffuse Transmittance Spectrometry for infrared Microsampling 308 David J. J. Fraser, Kelly L. Norton, and Peter R. Griffiths, Department of Chemistry, University of California, Riverside, CA 92521-0403 Differentiation of Leucine and Isoleucine Residues in Peptides by Consecutive Reaction Mass Spectrometry 311 Takemichi Nakamura*, Hidemi Nagaki, Yasuko Ohki, and Takeshi Kinoshita, Analytical and Metabolic Research Laboratories, Sankyo Co., Ltd., 2-58, Hiromachi 1-Chome, Shinagawa-ku, Tokyo 140, Japan Continuous On-Line Monitoring of Biomolecules Based on Automated Homogeneous Enzyme-Linked Competitive Binding Assays 314 Sylvia Daunert and Leonidas G. Bâchas*, Department of Chemistry, University of Kentucky, Lexington, KY 40506-0055 and Genevieve S. Ashcom and Mark E. Meyerhoff, Department of Chemistry, The University of Michigan, Ann Arbor, MI 48109-1055
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Polishable and Robust Biological Electrode Surfaces 318 Joseph Wang* and Kurian Varughese, Department of Chemistry, New Mexico State University, Las Cruces, NM 88003
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