GC-MS法测定人尿液中甲基苯丙胺的浓度

Determination of Methylamphetamine Concentration in Human Urine Sample by GC-MS

目的：建立测定人尿液中甲基苯雨胺浓度的方法。方法：取尿液样本2ml，加入0．1moYL氢氧化钠（Na0H）溶液调节其pH〉11，加入乙酸乙酯，进行液．液萃取，取乙酸乙酯层加热浓缩，最后取1μl浓缩液进样。采用气-质联用（GC—MS）法测定，以选择离子检测扫描（SIM）模式进行定量分析，选择离子为m／z58．91。结果：甲基苯丙胺尿药浓度在0．5-20μg／ml浓度范围线性关系良好（r=0．9934），最低检测限为0．05μg／ml；日内、日间RSD〈5％，平均回收率为106％-109％。结论：本方法快速、准确、重复性好，可用于尿液样本中甲基苯丙胺浓度的测定。

OBJECTIVE： To establish the method for the determination of methylamphetamine concentration in human urine sample. METHODS： 2 ml of urine sample was added into 0.1 mol/L NaOH and then pH was〉11, and the sample was extracted by liquid-liquid solvent extraction with ethyl acetate. The solution in ethyl acetate layer was concentrated by heating. 1 μl of concentrate was sampled and analyzed quantitatively by GC-MS. SIM mode was adopted for quantitative analysis. RESULTS： The linear range of methylamphetamine were 0.5-20μg/ml （r=0.993 4）, and the lowest detectable limit was 0.05 μg/ml; RSD of inter-day and intra-day tests were lower than 5%, and average recoveries were 106%-109%. CONCLUSIONS： The developed method is sensitive, rapid, accurate with good reproducibility, and is suitable for the content determination of methylamphetamine in urine sample.