Gan B K, Baugh D, Liu R H, Walia A S
Department of Criminal Justice, University of Alabama, Birmingham.
J Forensic Sci. 1991 Sep;36(5):1331-41.
A rapid and effective solid-phase extraction procedure using Bond Elute Certify bonded silica sorbent cartridges was adopted to extract amphetamine, methamphetamine, and 3,4-methylenedioxymethamphetamine (MDMA or Ecstasy) from urine samples. The extract was derivatized with trichloroacetic anhydride prior to gas chromatography/mass spectrometry (GC/MS) analysis with selected ion monitoring of the following ions: 190, 91, 188; 204, 91, 202; 162, 135, 202; 194, 123; and 211, 209 for the derivatized amphetamine, methamphetamine, MDMA, d5-amphetamine, and d9-methamphetamine, respectively. The first of the ions listed for each compound was used for quantitation. The compound d5-amphetamine was used as the internal standard for amphetamine, and d9-methamphetamine was used for methamphetamine and MDMA. Results showed a higher than 65% recovery and a reproducibility with less than a 5% coefficient of variation. When a sample size of 2 mL was used, the lowest detectable concentration was about 50 ng/mL, and a near-perfect fit can be obtained (within the 250 to 4000-ng/mL concentration range studied) using a second-order polynomial model.
采用使用Bond Elute Certify键合硅胶吸附剂小柱的快速有效固相萃取程序，从尿液样本中提取苯丙胺、甲基苯丙胺和3,4-亚甲基二氧基甲基苯丙胺（摇头丸）。提取物在进行气相色谱/质谱（GC/MS）分析前，用三氯乙酸酐衍生化，采用选择离子监测以下离子：衍生化苯丙胺的190、91、188；甲基苯丙胺的204、91、202；摇头丸的162、135、202；d5-苯丙胺的194、123；以及d9-甲基苯丙胺的211、209。每种化合物列出的第一个离子用于定量。化合物d5-苯丙胺用作苯丙胺的内标，d9-甲基苯丙胺用作甲基苯丙胺和摇头丸的内标。结果显示回收率高于65%，变异系数小于5%，具有良好的重现性。当使用2 mL样本量时，最低检测浓度约为50 ng/mL，使用二阶多项式模型（在所研究的250至4000 ng/mL浓度范围内）可获得近乎完美的拟合。
