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目的:建立人体尿液中曲马多的SPE-GC-MS定性定量检测分析方法。方法:人体尿液样本采用固相萃取法进行提取,用BSTFA+1%TMCS试剂衍生后,用气相色谱-质谱仪在电子电离模式下检测样本中的曲马多,通过同位素内标方法进行定量分析,从线性、抗干扰性、精密度、回收率及稳定性等方面对方法进行验证;收集临床样本,经本方法同时比对免疫层析法进行临床分析比对。结果:方法的最低检出量为2.0 ng/mL;定量线性范围为75.0~600.0 ng/mL,,最低定量限为150.0 ng/mL;在100.0和450.0 ng/mL的浓度下的日内精密度分别为3.90%和1.13%(n=6),日间精密度为1.02%和0.72%(n=6);在150.0和300.0 ng/mL浓度下,前处理回收率分别为95.73%和100.75%(n=3);临床用尿液免疫层析法筛选出来的11份临床阳性尿液样本及1例阴性样本,经本方法及尿液免疫层析法进行检测,结果一致。结论:本方法是一种准确、灵敏、特异性好的检测方法,可用于涉毒人员尿液中曲马多的定性定量分析。
Objective: To establish a qualitative and quantitative detection and detection method of tramadol in human urine by SPE-GC-MS. METHODS: Human urine samples were extracted by solid-phase extraction. After derivatization with BSTFA + 1% TMCS reagent, the amount of tramadol was determined by gas chromatography-mass spectrometry in the ionization mode and quantified by isotope internal standard method Analysis, from the linear, anti-interference, precision, recovery and stability of the method validation; clinical samples collected by the method at the same time compared to immunochromatographic clinical analysis and comparison. Results: The minimum detection limit was 2.0 ng / mL, the linear range was 75.0-600.0 ng / mL, and the lowest limit of quantification was 150.0 ng / mL. The intra-day precision at 100.0 and 450.0 ng / mL was Were 3.90% and 1.13% respectively (n = 6) with intraday precision of 1.02% and 0.72% (n = 6). The recoveries at pretreatment concentrations of 150.0 and 300.0 ng / mL were 95.73% and 100.75%, respectively n = 3). Clinically, 11 clinically positive urine samples and 1 negative sample were screened by urine immunochromatography. The results were consistent with the results of this method and urine immunochromatography. Conclusion: This method is an accurate, sensitive and specific detection method, which can be used for qualitative and quantitative analysis of tramadol in the urine of drug-related persons.