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Confirmation of Hormones in Animal Serum by Liquid Chromatography/Tandem Mass Spectrometry According to European Commission Decision 2002/657

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A novel and rapid method was developed and validated for the confirmation of endogenous and synthetic hormones in animal serum using LC/MS/MS. Detection of 17 -estradiol and -testosterone below the respective European Union-recommended levels of 0.1 and 0.5 g/L was achieved, as was a required performance level of 0.1 g/L for 17 -estradiol and 0.5 g/L for 17 -testosterone, medroxyprogesterone-17-acetate, and progesterone. The method was established with dilution of serum followed by ion-exchange SPE, LC separation and MS detection with electrospray ionization, selected reaction monitoring, and positive/negative switching. Two characteristic transitions were monitored for each analyte. The method was applied to bovine, ovine, porcine, equine, and avian samples and validated according to European Commission Decision 2002/657/EC and accepted for ISO/IEC 17025:2005 accreditation. An extended calibration curve allows naturally occurring levels of endogenous hormones to be quantified. Recoveries ranged from 97.3 for 17 -testosterone to 102.0 for 17 -estradiol. The decision limit CC ranged from 0.02 g/L for 17 - and -estradiol to 0.12 g/L for progesterone. Detection capability CC ranged from 0.03 g/L for 17 -estradiol to 0.20 g/L for progesterone.
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Document Type: Research Article

Affiliations: 1: Central Meat Control Laboratory, Department of Agriculture, Backweston Campus, Celbridge, Co. Kildare, Republic of Ireland. 2: State Laboratory, Backweston Campus, Young's Cross, Celbridge, Co. Kildare, Republic of Ireland.

Publication date: 2010-01-01

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  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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