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

• Published in: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Vol. 1187; p. 123048
• Main Authors: Gheddar, Laurie, Raul, Jean-Sébastien, Kintz, Pascal
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 15.12.2021; Elsevier
• Subjects: Anabolic Agents - analysis; Androgen Antagonists - analysis; androgens; buffer index; chemical species; Chromatography, High Pressure Liquid - methods; Doping in Sports; Hair; Hair - chemistry; hairs; HRMS; Humans; Internet; Life Sciences; Limit of Detection; Linear Models; liquid chromatography; liquids; Modulator metabolic; phosphates; Reproducibility of Results; SARMs; sports; Substance Abuse Detection; tandem mass spectrometry; Tandem Mass Spectrometry - methods; Toxicology; UHPLC-MS/MS; Hair; HRMS; SARMs; Modulator metabolic; UHPLC-MS/MS
• ISSN: 1570-0232; 1873-376X; 1873-376X
• DOI: 10.1016/j.jchromb.2021.123048

•Development and validation of a rapid method for SARMs in hair using UHPLC-MS/MS.•Simultaneous analysis of 9 SARMs and 2 metabolic modulators in hair.•First identification of S23 in authentic human hair in a doping case. 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-D4 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.