Anal. Chem. 1903, 5 5 , 157-160
Registry No. Carbon, 7440-44-0; radon, 10043-92-2;toluene, 108-88-3. LITERATURE C I T E D (1) Lucas, H. F. Rev Sci. Instrum. 1957,28, 60. (2) Prichard. H. M. Heafih Phys ., In press.
(3) Palmes, E. D.; Gunniso8nl,A. F. Am. Ind. Hyg. Assoc. J. 1973, 3 4 , 78.
157
(4) Weigel, F. Chem.-Ztg. 1978, 102, 287-299. (5) Altshuler, B.; Pasternack, B. Health Phys . 1983, 9 , 293.
RECEIVED for review July 30, 1982. Accepted September 29, 1982. This work was supported in part by-Grant No. ES01742-02 from the Institute Of Health Sciences.
Screening Method for Aroclor 1254 in Whole Blood Shane S. Que Hee," Jerry A. Ward, M. Wilson Tabor, and Raymond R. Suskind The Kettering Laboratory, University of Cincinnati Medical Center, 3223 Eden Avenue, Cincinnati, Ohio 45267
Polychlorinated biphenyls (PCBs) hawe been utilized as nonflammable and heat resistant oils in such articles as electrical transformers, condensers, and paint since 1930 ( I ) . They are ubiquitous in the biosphere (2, 3 ) . They have achieved some notoriety in the "Yusho" episode in Japan in 1968 ( 3 ) and more recently in Taiwan in 1979 (4, 5 ) . As of November 1, 1979, use of PCBs in new heat transfer systems in US. factories manufacturing or processing food, drugs, and cosmetics was no longer authorized. Use in electromagnets, transformers, and heat transfer and hydraulic systems is permitted until July 1, 1984 (6). Defective fluorescent light ballasts also emit PCBs contributing t o office air pollution (7). Thus, occupational and environmental exposures to PCBs will still occur into the future, and determination of PCBs En workers' blood ( 8 , 9 )wiill continue to be a valuable measure of PCB exposure. The methods for separation and quantification of polychlorinated biphenyls in serum or whole blood usually involve alkaline hydrolysis, hexane extraction, aind silica gel column chromatography of the concentrate of the hexane extraction (4,9,10). These methods are generally time-consuming and tedious: the extractions are usually multiple; the many concentrative steps may lead to losses by volatilization and adsorption; any impurities, in the solvents also are concentrated, limiting sensitivity or confounding GC/MS identification. In addition, incomplete documentation of the gel type may lead to irreproducible separations from investigator to investigator. There is a need for a semiquantitative quick-screening method to estimate PClBs in blood or serum. Such a method would be valuable to (assess if further chromatography is necessary for quantification or GC/MS analysis. Aroclor 1254 was the PCB chosen for this study since it is probably the most ubiquitous PCB (9). EXPERIMENTAL S E C T I O N Optimized Procedure. All glassware including syringes and tubes to be utilized in collecting blood was soaked in chromic acid overnight and rinsed (five times) in order: Type I distilled water a~ defined by the U.S. EF'A (11),acetone (Fisher Pesticide Grade A-40), Type I distilled water, hexane (Fisher Pesticide Grade H-300). Blood was drawn through a polyethylene butterfly valve. The fist 70 mL was discarded to minimize contamination in the event of later GC/MS. Blood (approximately 10 mL) was collected in preweighed 50-mL Kimalx 14-930 10A tubes fitted with Teflonlined screw caps and containing 200 USP units of heparin in 0.2 mL of aqueous isotonic saline. The heparin-containingtubes were shaken gently as the blood was collected to prevent clotting. The samples were then placed in a polystyrene refrigerated box (4-5 "C) in which the samples were transported to the laboratory, where they were stored (at 4-5 "C until analysis. Each blood sample was allowed to equilibrate to room temperature. The total weight was then recordled. A known weight 0003-2700/83/0355-0157$0 1.50/0
(ca. 5.0 f 0.1 g) of potassium hydroxide pellets (Fisher P-250) was added. Absolute ethanol (2.5 mL) was added by a prerinsed pipet. The caps were screwed on tightly and the tubes shaken until all the potassium hydroxide was dissolved. The solution will become hot but should not foam. The solution was digested at 90 "C for 1h in a water bath. With the capless tubes still in the bath, the ethanol was evaporated by blowing nitrogen over the surface of the solution for 10 min using a Pasteur pipet connected by Teflon tubing to a cylinder of compressed nitrogen. The solution was removed from the bath and allowed to cool. Pesticide Grade hexane (10 mL) was added (pipet),the caps were screwed on tightly, and the tubes were vigorously shaken for at least 15 separate shakes. The layers were allowed to separate for at least 10 min, or until no opacity was evident. An aliquot (10 wL) was then injected into the gas chromatograph to complete the screening phase. The column used for gas chromatographicanalyses was a 1.87 m X 6 mm 0.d. X 2 mm id. Pyrex column packed with 3% OV-101 on 100/120 mesh Chromosorb W-HP. A 63Nielectron capture (EC) detector was utilized in a Hewlett-Packard 5730-A gas chromatograph. The temperatures were 250 "C (injector), 203 "C (column), and 250 "C (detector). The flow of 95% argon/ methane was 25.0 k 1.5 mL/min. After 16 min the column temperature was raised to 250 "C for 30 min to allow elution of other blood compounds. A Hewlett-Packard Reporting Integrator (HP-3390A) was utilized to visualize and quantitate the peak areas. Preliminary examination of many blood samples revealed that the Aroclor 1254 pattern at low concentrations (
