steroids;
urine;
tandem mass spectrometry;
electrospray;
D O I:
10.1016/S0003-2670(02)00750-X
中图分类号:
O65 [分析化学];
学科分类号:
070302 ;
081704 ;
摘要:
The ban on the use of anabolic steroids as growth promoters in animal husbandry continues to be the policy of the European Union (EU). This requires National Reference Laboratories to provide analytical strategies capable of sustaining consumer confidence. The draft Sanco document 1085/2000 requires analytical methods to adhere to and meet pre-set performance characteristics. Here, we report the development of a semi-automated quantitative method capable of the screening and confirmation of 22 steroids in urine at one time. Screening is based on enzymatic deconjugation followed by dual solid phase extraction and subsequent off-line reversed phase liquid chromatography (LC)-electrospray tandem mass spectrometry (MS-MS). Simultaneous fraction collection of the split electrospray effluent makes available clean extracts. Suspect hormones present in these dried fractions are confirmed either by further electrospray MS-MS, incorporating additional transitions or by gas chromatography (GC) high-resolution MS after appropriate derivatisation. Validation results are presented for the screening assay together with the measured CCalpha and CCbeta values. The compatibility of the confirmation approach with European Union criteria is discussed for a level of 1 ng ml(-1) (C) 2002 Elsevier Science B.V. All rights reserved.