Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825, Japan.
Anal Chim Acta. 2010 Feb 19;661(1):42-6. doi: 10.1016/j.aca.2009.12.013. Epub 2009 Dec 16.
A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.
建立了一种用单块硅胶固相萃取小柱同时萃取和衍生尿液中苯丙胺（APs）和 3,4-亚甲二氧基苯丙胺（MDAs）的简单、灵敏、特异的气相色谱-质谱法。所有的程序，如样品加载、洗涤和洗脱，都通过离心来完成。尿液中的 APs 和 MDAs 被吸附在单块硅胶上，并在柱中与丙酰氯甲酸酯衍生化。氘代苯丙胺-d(5) 被用作内标。线性范围为 0.01-5.0 µg mL(-1) 对苯丙胺（MA）和 3,4-亚甲二氧基甲基苯丙胺（MDMA），0.02-5.0 µg mL(-1) 对苯丙胺（AP）和 3,4-亚甲二氧基苯丙胺（MDA）（相关系数> = 0.995）。尿液中 APs 和 MDAs 的回收率为 84-94%，含 0.1、1.0 和 4.0 µg mL(-1) APs 和 MDAs 的尿液样品的日内和日间重现性的相对标准偏差为 1.4%-13.6%。尿液中的最低检测限（信噪比> = 3）为 MA 和 MDMA 为 5 ng mL(-1)，AP 和 MDA 为 10 ng mL(-1)。该方法可用于在已加载少量溶剂的离心柱上同时进行萃取和衍生化。
