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目的:利用具有高分离效能和结构确证功能的液相色谱串联质谱来探索、建立毛发中兴奋剂(酯类、母体、代谢物)的检测和评价方法,并应用于运动员头发检测,为毛发的兴奋剂检测打下基础。方法:非脂类药物:称取50 mg头发,加入d3-睾酮作内标,使用蛋白酶K水解2小时,加入正戊烷/乙醚提取。三氯甲烷/异丙醇再次提取后两次有机相混合吹干,最后用甲醇/水和正己烷除去油脂,复溶后进样分析。酯类药物:50 mg头发,加内标以及水解方法同上,加入正戊烷提取,复溶后进样分析。结果与结论:方法验证中得出线性相关系数、最低检测限和最低定量限满足日常定量要求和头发中检测兴奋剂灵敏度的要求;药物日间精密度<20%,日内精密度<20%,回收率在50%以上;基质效应在80%～120%之间,符合一般验证要求。将建立的检测方法进行方法验证和评估后,应用于运动员头发中类固醇药物的检测。
OBJECTIVE: To explore and establish a method for the detection and evaluation of stimulants (esters, maternal and metabolites) in hair by using liquid chromatography tandem mass spectrometry (HPLC-MS / MS) with high separation efficiency and structural confirmation. The method is applied to hair testing of athletes Doping test laid the foundation. Methods: Non-lipid drugs: Weigh 50 mg of hair, add d3-testosterone as internal standard, use proteinase K for 2 hours and add n-pentane / ether for extraction. Chloroform / isopropanol extract again after the two organic phases were mixed and dried, and finally with methanol / water and n-hexane to remove grease, reconstituted sample analysis. Ester drugs: 50 mg hair, plus internal standard and hydrolysis method Ibid, adding n-pentane extraction, reconstituted injection analysis. RESULTS AND CONCLUSION: The linear correlation coefficient, the lowest detection limit and the lowest quantitation limit were obtained in the method validation to meet the daily quantitative requirements and the sensitivities of the test stimulants in hair. The intraday precision of the drug was less than 20% and the intraday precision was less than 20% The recovery rate is over 50%. The matrix effect is between 80% and 120%, which meets the general verification requirements. The established test method for method validation and evaluation, applied to the hair of athletes in the detection of steroid drugs.