摘要
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.
出处
《中国药房》
CAS
CSCD
2014年第30期2824-2825,共2页
China Pharmacy