Gas chromatographic determination of chloramphenicol residues in shrimp: interlaboratory study.
An interlaboratory study of a gas chromatographic method for determining chloramphenicol (CAP) residues in shrimp was conducted. An internal standard (Istd), the meta isomer of CAP, was added to the shrimp, and the treated shrimp were homogenized with ethyl acetate. The ethyl acetate extract was defatted with hexane, and the CAP was partitioned into ethyl acetate from an aqueous salt solution. The ethyl acetate was evaporated, and the dried residue was treated with Sylon, a trimethylsilyl derivatizing agent, to yield the trimethylsilyl derivative of CAP. A portion of the solution containing the derivative was injected into a gas chromatograph equipped with an electron capture detector. Levels of fortified and incurred CAP were calculated from the peak area ratio of standard CAP to Istd. Recoveries of CAP from tissue directly fortified at 5 ppb were 102% (within-laboratory relative standard deviation [RSDr] = 5.6%), 104% (RSDr = 5.5%), and 108% (RSDr = 6.3%) from Laboratories 1, 2, and 3, respectively. Incurred-CAP residues at 5 and 10 ppb levels were also determined, with the following results: Laboratory 1: composite A, 4.56 ppb (RSDr = 14.0%); composite B, 8.38 ppb (RSDr = 11.6%); Laboratory 2: composite A, 4.17 ppb (RSDr = 12.5%); composite B, 8.90 ppb (RSDr = 5.60%); Laboratory 3: composite A, 4.66 ppb (RSDr = 14.9%); composite B, 11.0 ppb (RSDr = 11.8%).
U.S. Food and Drug Administration, Animal Drugs Research Center, Denver, CO 80225-0087.
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RK
Munns
D C
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Holland
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Roybal
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JM
Storey
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Long
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Stehly
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SM
Plakas
D000818:Animals; D002701:Chloramphenicol / Q000032:analysis*; D002849:Chromatography, Gas / Q000379:methods* / Q000706:statistics & numerical data; D033364:Decapoda; D004350:Drug Residues; D015203:Reproducibility of Results; D014297:Trimethylsilyl Compounds
D014297:Trimethylsilyl Compounds; D002701:Chloramphenicol