Mandrioli Roberto, Mercolini Laura, Protti Michele
Department for Life Quality Studies (QuVi), Alma Mater Studiorum - University of Bologna, Corso d'Augusto 237, 47921 Rimini, Italy.
Research group of Pharmaco-Toxicological Analysis (PTA Lab), Department of Pharmacy and Biotechnology (FaBiT), Alma Mater Studiorum-University of Bologna, Via Belmeloro 6, 40126 Bologna Italy.
Molecules. 2020 Feb 26;25(5):1046. doi: 10.3390/molecules25051046.
Reliable, feasible analytical methods are needed for forensic and anti-doping testing of cocaine and its most important metabolites, benzoylecgonine, ecgonine methyl ester, and cocaethylene (the active metabolite formed in the presence of ethanol). An innovative workflow is presented here, using minute amounts of dried blood or plasma obtained by volumetric absorptive microsampling (VAMS), followed by miniaturized pretreatment by dispersive pipette extraction (DPX) and LC-MS/MS analysis. After sampling 20 µL of blood or plasma with a VAMS device, the sample was dried, extracted, and loaded onto a DPX tip. The DPX pretreatment lasted less than one minute and after elution with methanol the sample was directly injected into the LC-MS/MS system. The chromatographic analysis was carried out on a C8 column, using a mobile phase containing aqueous formic acid and acetonitrile. Good extraction yield (> 85%), precision (relative standard deviation, RSD < 6.0%) and matrix effect (< 12%) values were obtained. Analyte stability was outstanding (recovery > 85% after 2 months at room temperature). The method was successfully applied to real blood and plasma VAMS, with results in very good agreement with those of fluid samples. The method seems suitable for the monitoring of concomitant cocaine and ethanol use by means of plasma or blood VAMS testing.
在对可卡因及其最重要的代谢物苯甲酰芽子碱、芽子碱甲酯和可口乙酮(在有乙醇存在时形成的活性代谢物)进行法医和反兴奋剂检测时,需要可靠、可行的分析方法。本文介绍了一种创新的工作流程,使用通过体积吸收微采样(VAMS)获得的微量干血或血浆,随后通过分散移液器萃取(DPX)进行小型化预处理,并进行液相色谱 - 串联质谱(LC-MS/MS)分析。用VAMS装置采集20μL血液或血浆后,将样品干燥、萃取并加载到DPX小柱上。DPX预处理持续不到一分钟,用甲醇洗脱后,样品直接注入LC-MS/MS系统。色谱分析在C8柱上进行,使用含有甲酸水溶液和乙腈的流动相。获得了良好的萃取率(>85%)、精密度(相对标准偏差,RSD<6.0%)和基质效应(<12%)值。分析物稳定性出色(室温下2个月后回收率>85%)。该方法成功应用于实际的血液和血浆VAMS,结果与液体样品的结果非常吻合。该方法似乎适用于通过血浆或血液VAMS检测监测可卡因和乙醇的同时使用情况。