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采用 UHPLC-MS/MS 对 SARMs 和代谢调节剂进行筛选的开发和验证:在兴奋剂案例中的应用及对真实人发中 S23 的首次鉴定。

Development and validation of SARMs and metabolic modulators screening in hair using UHPLC-MS/MS: Application to a doping case and first identification of S23 in authentic human hair.

机构信息

Institut de médecine légale, 11 rue Humann, 67000 Strasbourg, France.

Institut de médecine légale, 11 rue Humann, 67000 Strasbourg, France.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2021 Dec 15;1187:123048. doi: 10.1016/j.jchromb.2021.123048. Epub 2021 Nov 17.

Abstract

Selective Androgen Receptors Modulators (SARMs) are a new class of doping drugs that emerged in sport since 2008. Easy access on the Internet also leads to their misuse by amateurs. It seems important for a laboratory of toxicology to develop a targeted screening of SARMs, given their health risks. A method has been developed and validated for the analysis in hair of 9 SARMs (AC262536, ACP-105, andarine, LGD-4033, MK-0773, MK 677, ostarine, RAD 410 and S23) and 2 other metabolic modulators (GW501516, SR9009), using liquid chromatography coupled to tandem mass spectrometry. After addition of bicalutamide-D used as internal standard and incubation in phosphate buffer pH = 9.5, 20 mg of hair samples were extracted with liquid/liquid extraction. Linearity was verified for all compounds between 0.5 and 50 and 2000 pg/mg. LOD and LOQ were determined between 0.1-20 and 0.5-50 pg/mg respectively, according to the various analytes. Intra- and inter-day precision (CV < 20%), matrix effects and recovery were evaluated for all compounds with CVs < 20%. The application and the interest of SARMs screening was demonstrated in a doping case. Three SARMs were detected namely andarine (120-1644 pg/mg), ostarine (1-9 pg/mg) and S23 (0.6-16 pg/mg) in 6x1 cm segments of the subject.

摘要

选择性雄激素受体调节剂(SARMs)是 2008 年以来运动中出现的一类新型兴奋剂。互联网的便捷访问也导致业余爱好者滥用这些药物。鉴于其健康风险,毒理学实验室似乎有必要开发针对 SARMs 的靶向筛选方法。已经开发并验证了一种用于分析头发中 9 种 SARMs(AC262536、ACP-105、andarine、LGD-4033、MK-0773、MK 677、ostarine、RAD 410 和 S23)和 2 种其他代谢调节剂(GW501516、SR9009)的方法,使用液相色谱-串联质谱法。在添加作为内标物的比卡鲁胺-D 并在 pH=9.5 的磷酸盐缓冲液中孵育后,用液/液萃取法提取 20 毫克的头发样本。所有化合物在 0.5 到 50 和 2000 pg/mg 之间均具有线性。根据各种分析物,LOD 和 LOQ 分别确定为 0.1-20 和 0.5-50 pg/mg。所有化合物的日内和日间精密度(CV<20%)、基质效应和回收率均进行了评估,CV 值均<20%。在一个兴奋剂案例中证明了 SARMs 筛选的应用和意义。在 6x1 厘米的受试者头发样本中检测到了三种 SARMs,分别为 andarine(120-1644 pg/mg)、ostarine(1-9 pg/mg)和 S23(0.6-16 pg/mg)。

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