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对尿中痕量蛋白同化激素药物去氢甲睾酮(大力补)的净化富集及其内标物选择进行了探讨。建立了以XAD-2富集样品,酶水解后碱性条件乙醚提取,以炔雌醇为内标物,制成TMS-衍生物后,采用GC-MS,多离子检测方式(MID)测定的方法。该法快速、灵敏、专属。XAD-2富集样品回收率大于85%,CV小于7%,尿药浓度在0.02～0.30 μg/ml呈线性关系,最低检测尿药浓度为20 ng/ml。实验结果表明,尿中内源性物质对大力补及其代谢物测定均无干扰。利用质谱及多离子色谱证明大力补的主要代谢物为6-β-羟基大力补,服药后94 h代谢物仍可被检出,本法已成功地用于真实尿样的分析。
The purification and enrichment of urinary trace protein anabolic hormone dehydrogenated methyltestosterone (Dacoxib) and its internal standard selection were discussed. A method was developed for the determination of TMS-derivatives by XAD-2 enrichment, enzymatic hydrolysis with ether and extraction with ethinyl estradiol as internal standard. The TMS-derivatives were determined by GC-MS and multi-ion detection method. The method is fast, sensitive and exclusive. The recovery rate of XAD-2 enriched samples was more than 85%, the CV was less than 7%, the urinary drug concentration was linear with 0.02-0.30 μg / ml, and the lowest urinary drug concentration was 20 ng / ml. The experimental results show that urine endogenous substances to vigorously make up and its metabolites determination without interference. Mass spectrometry and multi-ion chromatography proved that the main metabolite of Herba Daphnia was 6-β-Hydroxysuccopurine, which could still be detected after 94 h. This method has been successfully applied to the real urine samples.