Veterinary Laboratory of Serres, Terma Omonoias, Serres 62110, Greece.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jan 15;879(2):225-9. doi: 10.1016/j.jchromb.2010.11.029. Epub 2010 Dec 3.
In the present paper we report the LC-MS/MS determination of residues of 12 anabolic steroids in bovine serum, as an expansion of our work protocols for steroids determination in biological matrices. Steroids analyzed included α-zearalanol, β-zearalanol, α-trenbolone, β-trenbolone, methyltestosterone, α-estradiol, β-estradiol, ethynylestradiol, α-boldenone, β-boldenone, α-nortestosterone and β-nortestosterone. Following protein precipitation, serum samples were cleaned up by solid-phase extraction using Oasis HLB and Amino cartridges. Atmospheric pressure chemical ionization (APCI) in both positive and negative ionization modes was used and mass spectrometry detection was carried out in multiple reaction monitoring mode following two or (in most cases) three product ions per precursor ion. The method was validated in accordance with the Commission Decision 2002/657/EC. The decision limit (CCα) values obtained, ranged from 0.01 to 0.07 ng/ml and the detection capability (CCβ) values obtained ranged from 0.02 to 0.12 ng/ml. The recoveries ranged from 70.2% to 118.2%. The developed method is suitable for routine and confirmatory purposes such as control of illegal use in livestock production.
在本论文中，我们报告了采用 LC-MS/MS 法测定牛血清中 12 种同化甾类激素残留量的方法，这是我们在生物基质中进行类固醇检测工作方案的扩展。分析的类固醇包括α-玉米赤霉醇、β-玉米赤霉醇、α-群勃龙、β-群勃龙、甲基睾酮、α-雌二醇、β-雌二醇、乙炔雌二醇、α--boldenone、β-boldenone、α-去甲睾酮和β-去甲睾酮。采用蛋白沉淀法，使用 Oasis HLB 和 Amino 小柱进行固相萃取净化，然后采用大气压化学电离（APCI）正、负离子模式进行检测，在多反应监测模式下对每个前体离子进行两次或（大多数情况下）三次产物离子检测。该方法按照欧盟委员会 2002/657/EC 号决议进行验证。得到的检测限（CCα）值范围为 0.01-0.07ng/ml，得到的检测能力（CCβ）值范围为 0.02-0.12ng/ml。回收率范围为 70.2%-118.2%。所建立的方法适用于常规和确证目的，如控制畜牧业中非法使用。
