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采用 UPLC-MS-MS 检测和 UPLC-q-TOF-MS 确证毛发中采集的五个不同解剖部位的司坦唑醇。

Testing for Stanozolol, Using UPLC-MS-MS and Confirmation by UPLC-q-TOF-MS, in Hair Specimens Collected from Five Different Anatomical Regions.

机构信息

Institut de Médecine Légale, 11 rue Humann, Strasbourg 67000, France.

X-Pertise Consulting, 42 rue Principale, 67206 Mittelhausbergen, France.

出版信息

J Anal Toxicol. 2020 Dec 12;44(8):834-839. doi: 10.1093/jat/bkaa023.

DOI:10.1093/jat/bkaa023
PMID:32128595
Abstract

An athlete challenged the result from an in-competition doping test which returned with an adverse analytical finding for stanozolol, claiming it was due to supplement contamination. Her lawyer asked the laboratory to analyze several hair specimens simultaneously collected from five different anatomical regions, head, arm, leg, pubis and armpit, to document the pattern of drug exposure. A specific UPLC-MS-MS method was developed. After decontamination with dichloromethane, stanozolol was extracted from hair in the presence of stanozolol-d3 used as internal standard, under alkaline conditions, with diethyl ether. Linearity was observed for concentrations ranging from 5 pg/mg to 10 ng/mg. The method has been validated according to linearity, precision and matrix effect. Concentrations of stanozolol in head hair, pubic hair, arm hair, leg hair and axillary hair were 73, 454, 238, 244 and 7,100 pg/mg, respectively. The concentration of stanozolol in head hair is in accordance with data published in the literature. When comparing the concentrations, body hair concentrations were higher than the concentration found in head hair. These results are consistent with a better incorporation rate of stanozolol in body hair when compared to head hair. The simultaneous positive concentrations in different hair types confirm the adverse analytical finding in urine of the top athlete, as the measured concentrations do not support the theory of contamination. For the first time, an anabolic agent was simultaneously tested in hair collected from five different anatomical regions from the same subject, with a large distribution of concentrations, due to anatomical variations, and these findings will help interpretation in further doping cases when documented with hair.

摘要

一位运动员对比赛中的兴奋剂检测结果提出质疑,该结果显示司坦唑醇检测呈阳性,运动员声称这是由于补充剂污染所致。她的律师要求实验室同时分析从五个不同解剖区域(头部、手臂、腿部、阴部和腋窝)采集的几根头发样本,以记录药物暴露的模式。开发了一种特定的 UPLC-MS-MS 方法。在用二氯甲烷进行去污后,在碱性条件下,用二乙醚提取头发中的司坦唑醇,并加入司坦唑醇-d3 作为内标。在 5pg/mg 至 10ng/mg 的浓度范围内观察到线性。该方法已根据线性、精密度和基质效应进行了验证。在头部、阴部、手臂、腿部和腋窝头发中,司坦唑醇的浓度分别为 73、454、238、244 和 7100pg/mg。头部头发中司坦唑醇的浓度与文献中公布的数据一致。当比较浓度时,身体毛发的浓度高于头部头发中发现的浓度。这些结果与身体毛发中司坦唑醇的更好掺入率一致,与头部毛发相比。不同头发类型中同时存在阳性浓度证实了顶尖运动员尿液中的分析性兴奋剂检测结果,因为所测量的浓度不支持污染理论。这是第一次在同一受试者的五个不同解剖区域同时测试来自不同部位的头发,由于解剖学上的差异,浓度分布广泛,这些发现将有助于在进一步的兴奋剂案例中进行解释,当用头发记录时。

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