Paterson S, Cordero R, McCulloch S, Houldsworth P
Toxicology Unit, Imperial College School of Medicine, London, UK.
Ann Clin Biochem. 2000 Sep;37 ( Pt 5):690-700. doi: 10.1258/0004563001899744.
A method for the simultaneous analysis of urine for the major drugs of abuse is described. The analytical procedure uses solid-phase extraction (SPE), gas chromatography-mass spectrometry (GC-MS) and a semi-automated identification process. It allows simultaneous extraction, derivatization and analysis of acidic, neutral and basic drugs from urine. Urine samples were subjected to enzymatic hydrolysis followed by SPE using Bakerbond narc-2 columns. The eluant was selectively derivatized with N-methyl-bis-trifluoroacetamide (MBTFA) and N-methyl-N-trimethylsilyltrifluoroacetamide + 1% trimethylchlorosilane. Analysis was performed using a GC-MS system operating in full scan mode. A simple macro programme was written to enhance the mass spectra identification capabilities of the MS software by producing extracted ion chromatograms (EIC) for the drugs of interest. Once a suspect compound was indicated by EIC, the mass spectrum of the compound was searched manually against reference libraries for positive identification and the retention time checked against that of the standard. This procedure has increased both the amount and the reliability of information given to clinicians without increasing the cost per sample. The system has been in routine operation for 24 months, processing up to 40 urine samples per day, with a usual turn-around time of 48 h.
本文描述了一种同时分析尿液中主要滥用药物的方法。该分析程序采用固相萃取（SPE）、气相色谱 - 质谱联用（GC - MS）以及半自动鉴定过程。它能够同时从尿液中萃取、衍生化并分析酸性、中性和碱性药物。尿液样本先进行酶解，然后使用Bakerbond narc - 2柱进行固相萃取。洗脱液用N - 甲基 - 双（三氟乙酰胺）（MBTFA）和N - 甲基 - N - （三甲基硅烷基）三氟乙酰胺 + 1% 三甲基氯硅烷进行选择性衍生化。使用在全扫描模式下运行的GC - MS系统进行分析。编写了一个简单的宏程序，通过生成感兴趣药物的提取离子色谱图（EIC）来增强质谱软件的质谱鉴定能力。一旦EIC显示有可疑化合物，将该化合物的质谱与参考库进行手动比对以进行阳性鉴定，并将保留时间与标准品的保留时间进行核对。该程序在不增加每个样本成本的情况下，增加了提供给临床医生的信息量和信息可靠性。该系统已常规运行24个月，每天处理多达40个尿液样本，通常周转时间为48小时。
