School of Pharmaceutical Sciences of Ribeirao Preto, University of São Paulo, Av. do Café s/n, Ribeirão Preto, São Paulo 14040-903, Brazil.
The Atomic Medicine Initiative, University of Technology Sydney, 15 Broadway, Ultimo, NSW 2007, Australia.
J Anal Toxicol. 2023 Jan 24;46(9):991-998. doi: 10.1093/jat/bkab116.
Urine is initially collected from athletes to screen for the presence of illicit drugs. Sweat is an alternative sample matrix that provides advantages over urine including reduced opportunity for sample adulteration, longer detection-time window and non-invasive collection. Sweat is suitable for analysis of the parent drug and metabolites. In this study, a method was developed and validated to determine the presence of 13 amphetamine- and cocaine-related substances and their metabolites in sweat and urine using disposable pipette extraction (DPX) by gas chromatography coupled to mass spectrometry. The DPX extraction was performed using 0.1 M HCl and dichloromethane:isopropanol:ammonium hydroxide (78:20:2, v/v/v) followed by derivatization with N-methyl-N-(trimethylsilyl) trifluoroacetamide at 90°C for 20 min. DPX extraction efficiencies ranged between 65.0% and 96.0% in urine and 68.0% and 101.0% in sweat. Method accuracy was from 90.0% to 104.0% in urine and from 89.0% to 105.0% in sweat. Intra-assay precision in urine and in sweat were <15.6% and <17.8%, respectively, and inter-assay precision ranged from 4.70% to 15.3% in urine and from 4.05% to 15.4% in sweat. Calibration curves presented a correlation coefficient -0.99 for all analytes in both matrices. The validated method was applied to urine and sweat samples collected from 40 professional athletes who knowingly took one or more of the target illicit drugs. Thirteen of 40 athletes were positive for at least one drug. All the drugs detected in the urine were also detected in sweat samples indicating that sweat is a viable matrix for screening or confirmatory drug testing.
尿液最初是从运动员身上采集的，用于筛查是否存在非法药物。汗液是另一种样本基质，与尿液相比具有优势，包括减少样本掺假的机会、更长的检测时间窗口和非侵入性采集。汗液适用于分析母体药物及其代谢物。在这项研究中，开发并验证了一种使用一次性移液管提取（DPX）结合气相色谱-质谱法测定汗液和尿液中 13 种苯丙胺和可卡因相关物质及其代谢物的方法。DPX 提取使用 0.1 M HCl 和二氯甲烷：异丙醇：氨水（78:20:2，v/v/v）进行，然后在 90°C 下用 N-甲基-N-（三甲基硅基）三氟乙酰胺衍生化 20 分钟。DPX 提取效率在尿液中为 65.0%至 96.0%，在汗液中为 68.0%至 101.0%。方法准确度在尿液中为 90.0%至 104.0%，在汗液中为 89.0%至 105.0%。尿液和汗液中的日内精密度均<15.6%和<17.8%，日内精密度范围分别为尿液中的 4.70%至 15.3%和汗液中的 4.05%至 15.4%。两种基质中所有分析物的校准曲线相关系数均为-0.99。该验证方法应用于 40 名职业运动员的尿液和汗液样本，这些运动员故意服用了一种或多种目标非法药物。40 名运动员中有 13 名至少有一种药物呈阳性。尿液中检测到的所有药物也在汗液样本中检测到，这表明汗液是筛查或确证药物检测的可行基质。
