Comprehensive automation of the solid phase extraction gas chromatographic mass spectrometric analysis (SPE-GC/MS) of opioids, cocaine, and metabolites from serum and other matrices
Comprehensive automation of the solid phase extraction gas chromatographic mass spectrometric analysis (SPE-GC/MS) of opioids, cocaine, and metabolites from serum and other matrices
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DOI：
10.1007/s00216-014-7815-7
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发表时间：
2014-07-01
影响因子：
4.3
通讯作者：
Daldrup, Thomas
中科院分区：
文献类型：
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作者：
Lerch, Oliver;Temme, Oliver;Daldrup, Thomas
分析血清中的阿片类药物、可卡因和代谢物是法医实验室的常规任务。通常，采用的方法包括许多手动或部分自动化的步骤，如蛋白质沉淀、稀释、固相萃取、蒸发和衍生化，然后进行气相色谱(GC)/质谱分析(GC/MS)或液相色谱(LC)/MS分析。在这项研究中，从一个经过验证的、部分自动化的常规方法发展出一种全面自动化的方法。这可以通过在自动化系统上复制方法参数来实现。只需要对参数进行边际优化。依靠x-y-z机器人进行人工蛋白质沉淀后的自动化包括固相萃取、洗脱液蒸发、衍生化(与N-甲基-N-三甲基硅三氟乙酰胺硅烷化)和进样GC/MS。对近170份正品血清样品和50多份其他基质(如尿液、不同组织和心脏血液)的正品可卡因、苯甲酰ecGonine、美沙酮、吗啡、可待因、6-单乙酰吗啡、二氢可待因和7-氨基氟硝西仑进行了定量分析，证明两种方法的分析结果甚至在接近定量限(低ng/ml范围)时都是相同的。据我们所知，这是文献中第一次报道使用这种样品制备系统的应用。
The analysis of opioids, cocaine, and metabolites from blood serum is a routine task in forensic laboratories. Commonly, the employed methods include many manual or partly automated steps like protein precipitation, dilution, solid phase extraction, evaporation, and derivatization preceding a gas chromatography (GC)/mass spectrometry (MS) or liquid chromatography (LC)/MS analysis. In this study, a comprehensively automated method was developed from a validated, partly automated routine method. This was possible by replicating method parameters on the automated system. Only marginal optimization of parameters was necessary. The automation relying on an x-y-z robot after manual protein precipitation includes the solid phase extraction, evaporation of the eluate, derivatization (silylation with N-methyl-N-trimethylsilyltrifluoroacetamide, MSTFA), and injection into a GC/MS. A quantitative analysis of almost 170 authentic serum samples and more than 50 authentic samples of other matrices like urine, different tissues, and heart blood on cocaine, benzoylecgonine, methadone, morphine, codeine, 6-monoacetylmorphine, dihydrocodeine, and 7-aminoflunitrazepam was conducted with both methods proving that the analytical results are equivalent even near the limits of quantification (low ng/ml range). To our best knowledge, this application is the first one reported in the literature employing this sample preparation system.