Sempio Cristina, Morini Luca, Vignali Claudia, Groppi Angelo
Department of Public Health, Experimental and Forensic Sciences, University of Pavia, via Forlanini 12, 27100 Pavia, Italy.
Department of Public Health, Experimental and Forensic Sciences, University of Pavia, via Forlanini 12, 27100 Pavia, Italy.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Nov 1;970:1-7. doi: 10.1016/j.jchromb.2014.08.039. Epub 2014 Sep 6.
The aim of the study was to develop and validate a simple, sensitive and specific method for the detection and quantitative determination of 88 substances among psychoactive drugs and their metabolites in whole blood, and to apply the procedure to postmortem cases. Samples were consecutively diluted with methanol, acetonitrile and mobile phase. All the molecules were separated and then identified through a liquid chromatographic, tandem mass spectrometric system, and eventually fully validated according to the international guidelines. The method proved to be highly sensitive and specific and all the validation parameters fulfilled the acceptance criteria. In particular linearity was studied in the range LOQ-1000 ng/mL; matrix effects and carry over were negligible and the majority of the compounds assessed to be stable over several freeze and thaw processes. Olanzapine is the most unstable compound. Protryptiline and flupenthixol did not fulfilled acceptance criteria, and although their transitions were kept on the instrumental settings, they were not considered for the fully validation. The method was applied to several postmortem cases, and the results were compared to the GC-MS systematic toxicological analysis currently in use in our laboratory, assessing to be a good complementary procedure and providing a better sensitivity. The LC-MS/MS method could be easily applicable to routine analyses of postmortem samples, as well as to a screening procedure for clinical purposes; however it should be carried out in combination with a general unknown screening method.
本研究的目的是开发并验证一种简单、灵敏且特异的方法,用于检测和定量全血中88种精神活性药物及其代谢物,并将该方法应用于死后案例。样品依次用甲醇、乙腈和流动相稀释。所有分子通过液相色谱-串联质谱系统进行分离和鉴定,并最终根据国际指南进行全面验证。该方法被证明具有高度灵敏性和特异性,所有验证参数均符合验收标准。特别是在定量限至1000 ng/mL范围内研究了线性;基质效应和残留可忽略不计,且评估的大多数化合物在多次冻融过程中稳定。奥氮平是最不稳定的化合物。普罗替林和氟哌噻吨未达到验收标准,尽管其跃迁保留在仪器设置中,但在全面验证中未予考虑。该方法应用于多个死后案例,并将结果与我们实验室目前使用的气相色谱-质谱系统毒理学分析进行比较,评估其为一种良好的补充方法且具有更高的灵敏度。液相色谱-串联质谱法可轻松应用于死后样品的常规分析以及临床目的的筛查程序;然而,它应与一般未知物筛查方法联合进行。