Institute of Legal Medicine, Forensic Toxicology Service, Faculty of Medicine, C/ San Francisco s/n, 15782 Santiago de Compostela, Spain.
Anal Bioanal Chem. 2011 Oct;401(7):2177-86. doi: 10.1007/s00216-011-5279-6. Epub 2011 Aug 7.
Robust and simple validated analytical methods are required in postmortem toxicology to confirm immunoassay screening analysis of drugs of abuse. In this work, microwave-assisted extraction (MAE) was evaluated as an alternative method for extraction of target compounds such as cocaine, benzoylecgonine, cocaethylene, morphine, codeine, 6-monoacetylmorphine, methadone, and 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine from vitreous humor. The MAE procedure parameters, namely, extraction temperature, time, and solvent volume, were optimized using a central composite design and applying desirability functions. The optimal conditions for extraction were 80 °C, 8 min, and 15 mL of dichloromethane solvent. The MAE-high-performance liquid chromatography-diode-array detection method was validated, showing its capability for the detection of concentrations in the range from 33 to 76 ng mL(-1) and recoveries in the range from 87 to 99.3% for all drugs. The MAE-based method was tested for 15 vitreous humor samples from forensic cases and its performance was compared with that of a solid-phase extraction method previously developed by our group. In general, better recovery and precision were achieved with the use of the MAE-based procedure.
在法医毒理学中，需要稳健且简单的经过验证的分析方法来确认对滥用药物的免疫分析筛选分析。在这项工作中，评估了微波辅助提取（MAE）作为从玻璃体液中提取目标化合物（如可卡因、苯甲酰古柯碱、古柯可因、吗啡、可待因、6-单乙酰吗啡、美沙酮和 2-亚乙基-1,5-二甲基-3,3-二苯基吡咯烷）的替代方法。使用中心组合设计和应用适宜性函数优化了 MAE 程序参数，即提取温度、时间和溶剂体积。提取的最佳条件为 80°C、8 分钟和 15 毫升二氯甲烷溶剂。验证了 MAE-高效液相色谱-二极管阵列检测方法，表明其能够检测 33 至 76ng/mL 范围内的浓度，所有药物的回收率在 87%至 99.3%之间。该 MAE 方法已用于 15 例法医案例的玻璃体液样本测试，并将其性能与我们小组先前开发的固相萃取方法进行了比较。一般来说，使用基于 MAE 的程序可以获得更好的回收率和精密度。
