Maresova Vera, Chadt Jiri, Novakova Eva
Institute of Forensic Medicine and Toxicology, First Faculty of Medicine, Charles University in Prague, Prague, Czech Republic.
Neuro Endocrinol Lett. 2008 Oct;29(5):749-54.
The purpose of this study is to develop the gas chromatographic-mass spectrometric method (GC-MS) for screening and semiquantification of drugs and drugs of abuse in human serum.
GC-MS method after liquid-liquid extraction (LLE) and derivatization with N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA) is presented for screening as well as identification and semiquantification of the most frequently used drugs and drugs of abuse in human serum.
Bovine serum spiked with ephedrine (EPHE), 3,4-methylenedioxymethamphetamine (MDMA), guaifenesin (GUAIF), tramadol (TRAM), phenobarbital (PHENO), amitriptyline (AMITR), cocaine (COCA), mirtazapine (MIRTA), dothiepin (DOTH), citalopram (CITAL), clomipramine (CLOMI), bromazepam (BMZPM), diazepam (DZPM), codeine (COD), morphine (MORPH), levomepromazine (LEVO), zolpidem (ZOLP), clozapine (CLOZP), alprazolam (ALPZM) was used for the recovery and repeatability study and for preparation of calibration curves of individual compounds or their TMS derivatives. Recoveries were tested on concentration levels 0.05, 0.1 and 0.5 microg/mL (n=6) and established in range 72.0-98.0%. Repeatabilities expressed as relative standard deviations (RSDs) measured at concentration levels 0.05, 0.1 and 0.5 microg/ mL (n=6) were lower than 10.0%. The calibration curves for analytes or their TMS derivatives were linear in concentration range 0.025-2.000 microg/mL (except of EPHE 2TMS, MDMA TMS, MORPH 2TMS, BMZPM TMS, ALPZM) with correlation coefficients exceeding 0.99. The limit of quantification (LOQ) for analytes used for evaluation study was 0.025 microg/mL (except analytes mentioned above).
The GC-MS method presented here is allowing screening, identification and semiquantification of the most commonly encountered drugs and drugs of abuse in human serum and can be successfully applied to analysis of real samples from clinical and forensic toxicology cases.
本研究旨在开发气相色谱 - 质谱法(GC-MS),用于筛查和半定量人血清中的药物及滥用药物。
介绍了液 - 液萃取(LLE)并用N - 甲基 - N - 三甲基硅烷基三氟乙酰胺(MSTFA)衍生后的GC-MS方法,用于筛查、鉴定和半定量人血清中最常用的药物及滥用药物。
用添加了麻黄碱(EPHE)、3,4 - 亚甲基二氧甲基苯丙胺(MDMA)、愈创甘油醚(GUAIF)、曲马多(TRAM)、苯巴比妥(PHENO)、阿米替林(AMITR)、可卡因(COCA)、米氮平(MIRTA)、多塞平(DOTH)、西酞普兰(CITAL)、氯米帕明(CLOMI)、溴西泮(BMZPM)、地西泮(DZPM)、可待因(COD)、吗啡(MORPH)、左美丙嗪(LEVO)、唑吡坦(ZOLP)、氯氮平(CLOZP)、阿普唑仑(ALPZM)的牛血清进行回收率和重复性研究,并制备各化合物或其TMS衍生物的校准曲线。在0.05、0.1和0.5μg/mL浓度水平(n = 6)下测试回收率,回收率范围为72.0 - 98.0%。在0.05、0.1和0.5μg/mL浓度水平(n = 6)下测得的以相对标准偏差(RSD)表示的重复性低于10.0%。分析物或其TMS衍生物的校准曲线在0.025 - 2.000μg/mL浓度范围内呈线性(EPHE 2TMS、MDMA TMS、MORPH 2TMS、BMZPM TMS、ALPZM除外),相关系数超过0.99。用于评估研究的分析物的定量限(LOQ)为0.025μg/mL(上述分析物除外)。
本文介绍的GC-MS方法可用于筛查、鉴定和半定量人血清中最常见的药物及滥用药物,并可成功应用于临床和法医毒理学案例的实际样本分析。