Determination of steroids in bovine hair: Validation of a microwave-assisted chemical derivatization method using liquid chromatography-tandem mass spectrometry and in vivo studies.,Drug Testing and Analysis

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Determination of steroids in bovine hair: Validation of a microwave-assisted chemical derivatization method using liquid chromatography-tandem mass spectrometry and in vivo studies.
Drug Testing and Analysis ( IF 2.6 ) Pub Date : 2020-06-30 , DOI: 10.1002/dta.2815
Diego G Rocha _{1,

2} , Mary Ane G Lana ₂ , Débora C S de Assis ₃ , Silvana V Cançado ₃ , Rodinei Augusti ₁ , Adriana F Faria ₁

Affiliation

Hair analysis has attracted great attention in the regulatory analysis of food‐producing animals, particularly due to the wider detection window of veterinary drugs in this matrix and also the possibility of confirming parent drugs with minimum metabolization. This work involved the development and validation of a quantitative liquid chromatography–tandem mass spectrometry method to determine 25 steroids and steroid esters in bovine hair. Sensitivity was improved using a fast and effective microwave‐assisted chemical derivatization with methoxyamine hydrochloride. The validation was conducted in accordance with the Decision 657/2002/EC guidelines. An animal experimentation procedure was performed on 12 bovine animals in which two commercial formulations containing boldenone undecylenate and testosterone propionate were administrated via intramuscular injections on the neck. The samples were collected for 78 days in which the detection of the administrated analytes was only observed near the application sites. For some of the monitored days, no analyte was detected on the neck area. Since the migration of the analytes was not observed in areas other than the application site, false‐negative results should be carefully considered when monitoring animal hair samples.

中文翻译：

牛毛中类固醇的测定：使用液相色谱-串联质谱和体内研究的微波辅助化学衍生方法的验证。

毛发分析在食品生产动物的法规分析中引起了极大的关注，特别是由于该基质中兽药的检测范围更广，并且有可能以最小的代谢率确定母体药物。这项工作涉及定量液相色谱-串联质谱法的开发和验证，该方法可测定牛毛中的25种类固醇和类固醇酯。使用盐酸甲氧基胺进行快速有效的微波辅助化学衍生，可以提高灵敏度。验证是根据657/2002 / EC决定指南进行的。对12只牛进行了动物实验，其中通过颈部肌肉注射施用了两种含有十一烯酸十一烯酮和丙酸睾丸酮的商业制剂。收集样品78天，其中仅在施用部位附近观察到施用的分析物的检测。在某些监控的日子里，在颈部区域未检测到任何分析物。由于在施药部位以外的其他区域未观察到分析物的迁移，因此在监测动物毛发样品时应仔细考虑假阴性结果。在颈部没有检测到分析物。由于在施药部位以外的其他区域未观察到分析物的迁移，因此在监测动物毛发样品时应仔细考虑假阴性结果。在颈部没有检测到分析物。由于在施药部位以外的其他区域未观察到分析物的迁移，因此在监测动物毛发样品时应仔细考虑假阴性结果。

更新日期：2020-06-30

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