响应面法优化-固相萃取-气相色谱法测定尿液中甲基苯丙胺

发布时间：2018-01-10 00:25

本文关键词：响应面法优化-固相萃取-气相色谱法测定尿液中甲基苯丙胺　出处：《理化检验(化学分册)》2013年10期 　论文类型：期刊论文

【摘要】：采用三因素三水平响应面分析法对尿液中甲基苯丙胺(MPM)的固相萃取(SPE)条件作优化试验,所得最佳SPE条件为:①尿样的酸度:pH 9.35(PBS);②上样速率:0.9 mL·min~(-1);③洗脱剂(乙酸乙酯)的用量:3.2 mL。所得淋出液氮吹蒸干,溶于100μL内标物(SKF_(525-A))乙醇溶液中,供气相色谱分析。用AB-5毛细管色谱柱分离,进样量为1μL。采用氮磷检测器进行测定。甲基苯丙胺的质量浓度与其峰面积在0.10~10.0 mg·L~(-1)范围内呈线性关系,检出限(3S/N)为0.062 mg·L~(-1)。日内和日间相对标准偏差(n=6)均小于5%。
[Abstract]:The solid phase extraction (SPE) conditions of methamphetamine (MPM) in urine were optimized by three factors and three levels response surface analysis. The optimum conditions of SPE were as follows: the acidity of the urine sample of 1: 1 was 9. 35% pH, and the pH of the urine sample was 9. 35%. (2) the sample rate was 0.9 mL 路min ~ (-1); (3) the amount of eluent (ethyl acetate): 3.2mL. the liquid nitrogen was evaporated and dissolved in the 100 渭 L internal standard (SKFD 525-An) ethanol solution. Gas supply phase chromatographic analysis. Separation by AB-5 capillary column. The concentration of methamphetamine was linear to its peak area in the range of 0.10 ~ 10.0 mg 路L ~ (-1) 路L ~ (-1). The detection limit of 3s / N was 0.062 mg 路L ~ (-1) 路L ~ (-1). The relative standard deviation (n ~ (6)) was less than 5 ~ (-1).
【作者单位】：山东中烟工业有限责任公司济南卷烟厂;吉林省公安厅物证鉴定中心;
【基金】：公安部重点研究计划项目(2010ZDYJJLST015)
【分类号】：D918.93;O657.71
【正文快照】： 甲站苯w胺(M A).俗称“冰箱”,已成为世界上滥用最为广泛的毒品丨随着此类海品滥川问题的丨I益严峻.对刑事技术部r j的要求也逐渐加大[2_1。固相萃取(SPE)技术由于操作简单、省力、节约溶剂》优势?lL成为临床毒物学和法庭每物学的药物分析中样品前处理方法的一个重要工具[5-

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