不同前处理模式下检验地芬尼多死亡结果比较

Comparison of the results of 4 death cases of difenidol under three different pretreatment modes

目的建立一种前处理优化条件下血中地芬尼多的液相色谱-串联质谱的检测方法。方法比较了血中三种不同的前处理方式(LLE、PP、SPE)的基质效应,采用液相色谱-串联质谱仪分析,多反应检测扫描模式(MRM)检测地芬尼多,采用外标法定量。结果采用SPE小柱的前处理方式最优。血中地芬尼多在1.0ng/m L~100ng/m L浓度范围内线性关系良好,回归方程为y=8.18×10^(4)x+18330(r=0.998),定量限在0.3ng/m L。地芬尼多在1ng/m L添加水平,回收率>95.0%,精密度<6.0%。结论本研究比较了几种不同的前处理方法,从中选择较为简便、基质干扰小的一种可用于血中地芬尼多的定性定量检测,同时测定了几起死亡案件中地芬尼多的血浓度,为侦查办案提供参考。

Objective To establish a method for the determination of difenidol in blood by Liquid chromatographytandem mass spectrometry under optimized conditions.Methods Three different pretreatment modes in blood were compared.Liquid chromatography-tandem mass spectrometer analysis was used.Difenidol was detected by multi reaction monitoring(MRM)mode and quantified by external standard method.Results The pretreatment of difenidol was the best by using SPE cartridge.Difenidol in blood has a good linear relationship in the concentration range of 1 ng/mL~100 ng/mL.The regression equation is y=8.18×10^(4)x+18330(r=0.998),and the limit of quantitation is 0.3 ng/mL.The recovery of difenidol which was added in blood at a level of 1 ng/mL was more than 95%and the relative standard deviation(RSD)was less than 6%.Conclusion This article compares several different pre-treatment modes,from which to select a relatively simple and little interference one can be used for qualitative and quantitative detection of difenidol in blood for case detection.