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首页> 外文期刊>Journal of mass spectrometry: JMS >Development, validation and application to real samples of amultiresidue LC-MS/MS method for determination of β_2-agonists and anabolic steroids in bovine hair
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Development, validation and application to real samples of amultiresidue LC-MS/MS method for determination of β_2-agonists and anabolic steroids in bovine hair

机译：多残留LC-MS / MS方法的开发，验证和在实际样品中的测定，用于测定牛毛中的β_2-激动剂和合成代谢类固醇

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β_2-agonists are often abused in cattle breeding because of their effects on animal growth and meat properties. The use of β_2-agonists as growth promoters is forbidden in the European Union (Council Directive 96/23/EC classifies them into group A of Annex I), due to their toxicity and carcinogenic properties, as for anabolic steroids,which are often administered in combination with β_2-agonists, to promote the storage of proteins and increase muscle size. A unique confirmatory liquid chromatography–tandem mass spectrometry (LC-MS/MS) method for the quantitative detection of 13 β_2-agonists and anabolic steroids plus the qualitative identification of other three analytes in bovine hair was developed and validated, according to Decision 2002/657/CE. Hair samples were washed with dichloromethane, digested within a NaOH solution and subjected to liquid–liquid extraction. The analysiswas performed by high performance liquid chromatography coupled to a triple quadrupolemass spectrometer operating in the selected reactionmonitoringmode. The absence of matrix interferents, together with good repeatability of both retention times and relative abundances of diagnostic transitions, allowed the correct identification of all analytes. The quantitative calibrations obtained from spiked blank hair samples proved linear in the range tested. CCα and CCβ ranged from0.5 ng/g to 30 ng/g. Intralaboratory reproducibility (CV%) ranged between 5.0 and 17.7 and trueness between 96%± 7% and 105%± 8%. The applicability of the method to real positive samples was demonstrated for both β_2-agonists and anabolic steroids. 17α-boldenone was found in most (70%) hair samples obtained from untreated animals, supporting the hypothesis of endogenous production of this steroid.
机译：β_2激动剂由于对动物生长和肉质的影响而经常在牛育种中滥用。由于它们的毒性和致癌特性，在欧盟中禁止将β_2激动剂用作生长促进剂（理事会指令96/23 / EC将它们归类为附件I的A组），因为它们通常具有合成代谢类固醇的毒性和致癌性。与β_2激动剂联用，可促进蛋白质的储存并增加肌肉大小。根据Decision 2002 / 657 / CE。头发样品用二氯甲烷洗涤，在NaOH溶液中消化，然后进行液-液萃取。该分析是通过高效液相色谱仪与以选定的反应监测模式运行的三重四极杆质谱仪耦合进行的。基质干扰物的不存在，以及保留时间和诊断转换的相对丰度都具有良好的可重复性，因此可以正确鉴定所有分析物。从加标的空白头发样品获得的定量校准证明在测试范围内呈线性。 CCα和CCβ的范围为0.5 ng / g至30 ng / g。实验室内可重复性（CV％）在5.0和17.7之间，真实性在96％±7％和105％±8％之间。证明了该方法对β_2-激动剂和合成代谢类固醇均适用于真实阳性样品。从未经治疗的动物中获得的大多数（70％）毛发样品中都发现了17α-boldenone，这支持了这种类固醇内源性产生的假说。

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