Foster B S, Gilbert D D, Hutchaleelaha A, Mayersohn M
Department of Chemistry, Northern Arizona University, Flagstaff 86011-5698, USA.
J Anal Toxicol. 1998 Jul-Aug;22(4):265-9. doi: 10.1093/jat/22.4.265.
An analytical method was developed for enantiomeric determination of amphetamine and methamphetamine in human urine. The enantiomers were isolated from urine by solid-phase extraction, and diastereomers were formed by derivatization with the chiral Marfey's reagent (1-fluoro-2,4-dinitrophenyl-5-l-aniline amide). The diastereomers were separated by reversed-phase high-performance liquid chromatography in a water/methanol mobile phase and detected by absorbance spectrophotometry at 340 nm. Linear standard curves were obtained for all four enantiomers over a concentration range of 0.16-1.00 mg/L in urine. The detection limit was 0.16 mg/L urine for each enantiomer, and the limit of quantitation was 0.40 mg/L. The urine of 10 decedents was analyzed by this method and by a previously published precolumn derivatization procedure using (-)-1-(9-fluorenyl)ethyl chloroformate (FLEC) as the derivatizing agent and fluorescence detection. Comparison of the results of the two methods by linear regression showed comparable results for both d-amphetamine and d-methamphetamine. Neither method detected the presence of the l-enantiomers in the urine samples.
建立了一种用于测定人尿中苯丙胺和甲基苯丙胺对映体的分析方法。通过固相萃取从尿液中分离对映体，并用手性Marfey试剂（1-氟-2,4-二硝基苯基-5-L-苯胺酰胺）衍生化形成非对映体。非对映体在水/甲醇流动相的反相高效液相色谱中分离，并在340nm处通过吸光分光光度法检测。在尿液中0.16-1.00mg/L的浓度范围内，所有四种对映体均获得了线性标准曲线。每种对映体的检测限为0.16mg/L尿液，定量限为0.40mg/L。用该方法和先前发表的以（-）-1-（9-芴基）乙基氯甲酸酯（FLEC）为衍生剂并进行荧光检测的柱前衍生化方法分析了10名死者的尿液。通过线性回归对两种方法的结果进行比较，结果表明d-苯丙胺和d-甲基苯丙胺的结果具有可比性。两种方法均未检测到尿液样品中L-对映体的存在。
