Determination and confirmation of pirlimycin residue in bovine milk and liver by liquid chromatography/thermospray mass spectrometry: interlaboratory study. 1996

D N Heller
U. S. Food and Drug Administration, Center for Veterinary Medicine, Beltsville, MD 20705, USA.

Three laboratories participated in trials of methods to determine and confirm pirlimycin residue in bovine milk and liver. The methods used liquid chromatography/thermospray mass spectrometry (LC/MS) with an internal standard to measure residue concentration. The internal standard was isopirlimycin, a stereoisomer of pirlimycin, which was resolved chromatographically. Determinative procedures were validated by replicate analyses of negative control, fortified control, and residue-incurred milk. For the milk method, average corrected recoveries (and coefficients of variation, CVs) were 83-113% (CV, 7.5-15.4%) at 0.2 ppm, 91-98% (CV, 3.4-18.5%) at 0.4 ppm, and 89-102% (CV, 8.8-22.9%) at 0.8 ppm. For the liver method, average corrected recoveries were 94-103% (CV, 2.2-7.1%) at 0.25 ppm, 87-94% (CV, 4.8-10.3%) at 0.5 ppm, and 96-101% (CV, 5.5-6.9%) at 1.0 ppm. There were no interferences in control samples of either matrix. Pirlimycin was confirmed by matching the retention time and relative abundances of 4 ions from sample extracts to corresponding values obtained for pirlimycin standard. Pirlimycin was confirmed in all residue-incurred samples and all samples fortified at regulatory tolerances (0.4 ppm in milk and 0.5 ppm in liver) by 2 of the 3 laboratories and in most samples by the third laboratory.

UI MeSH Term Description Entries
D008099 Liver A large lobed glandular organ in the abdomen of vertebrates that is responsible for detoxification, metabolism, synthesis and storage of various substances. Livers
D008892 Milk The off-white liquid secreted by the mammary glands of humans and other mammals. It contains proteins, sugar, lipids, vitamins, and minerals. Cow Milk,Cow's Milk,Milk, Cow,Milk, Cow's
D012015 Reference Standards A basis of value established for the measure of quantity, weight, extent or quality, e.g. weight standards, standard solutions, methods, techniques, and procedures used in diagnosis and therapy. Standard Preparations,Standards, Reference,Preparations, Standard,Standardization,Standards,Preparation, Standard,Reference Standard,Standard Preparation,Standard, Reference
D002417 Cattle Domesticated bovine animals of the genus Bos, usually kept on a farm or ranch and used for the production of meat or dairy products or for heavy labor. Beef Cow,Bos grunniens,Bos indicus,Bos indicus Cattle,Bos taurus,Cow,Cow, Domestic,Dairy Cow,Holstein Cow,Indicine Cattle,Taurine Cattle,Taurus Cattle,Yak,Zebu,Beef Cows,Bos indicus Cattles,Cattle, Bos indicus,Cattle, Indicine,Cattle, Taurine,Cattle, Taurus,Cattles, Bos indicus,Cattles, Indicine,Cattles, Taurine,Cattles, Taurus,Cow, Beef,Cow, Dairy,Cow, Holstein,Cows,Dairy Cows,Domestic Cow,Domestic Cows,Indicine Cattles,Taurine Cattles,Taurus Cattles,Yaks,Zebus
D002853 Chromatography, Liquid Chromatographic techniques in which the mobile phase is a liquid. Liquid Chromatography
D002981 Clindamycin An antibacterial agent that is a semisynthetic analog of LINCOMYCIN. 7-Chloro-7-deoxylincomycin,Chlolincocin,Chlorlincocin,Cleocin,Clindamycin Hydrochloride,Clindamycin Monohydrochloride,Clindamycin Monohydrochloride, Monohydrate,Dalacin C,7 Chloro 7 deoxylincomycin,Hydrochloride, Clindamycin,Monohydrate Clindamycin Monohydrochloride,Monohydrochloride, Clindamycin,Monohydrochloride, Monohydrate Clindamycin
D004350 Drug Residues Drugs and their metabolites which are found in the edible tissues and milk of animals after their medication with specific drugs. This term can also apply to drugs found in adipose tissue of humans after drug treatment. Drug Residue,Residue, Drug,Residues, Drug
D005504 Food Analysis Measurement and evaluation of the components of substances to be taken as FOOD. Analysis, Food,Analyses, Food,Food Analyses
D005506 Food Contamination The presence in food of harmful, unpalatable, or otherwise objectionable foreign substances, e.g. chemicals, microorganisms or diluents, before, during, or after processing or storage. Food Adulteration,Adulteration, Food,Adulterations, Food,Contamination, Food,Contaminations, Food,Food Adulterations,Food Contaminations
D000818 Animals Unicellular or multicellular, heterotrophic organisms, that have sensation and the power of voluntary movement. Under the older five kingdom paradigm, Animalia was one of the kingdoms. Under the modern three domain model, Animalia represents one of the many groups in the domain EUKARYOTA. Animal,Metazoa,Animalia

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