UAIL-DLLME-LC-MS/MS测定血液中地芬尼多与苯海拉明OA
Determination of Difenidol and Diphenhydramine in Blood Samples by Ultrasonic-assisted Ionic Liquid-based Dispersive Liquid-liquid Microextraction Coupled with LC-MS/MS
本研究拟建立血液中地芬尼多与苯海拉明的超声辅助离子液体-分散液液微萃取(ultrasonic-assisted ionic liquid dispersive liquid-liquid microextraction,UAIL-DLLME)-液相色谱串联质谱检测方法(liquid chromatography-tandem spectrometry,LC-MS/MS),为地芬尼多与苯海拉明相关案件的法医学鉴定提供参考.以1-丁基-3-甲基咪唑六氟磷酸盐([Bmim][PF6])为萃取剂,丙酮为分散剂,样品采用ZORBAX Eclipse Plus C18 RRHD色谱柱分离,流动相A为含0.1％甲酸的水溶液,流动相B为甲醇,采取梯度洗脱模式,流速为0.2 mL/min,电喷雾离子源(ESI+),采用多反应监测模式(multiple reaction monitoring,MRM)进行检测.血液中苯海拉明与地芬尼多的检出限均为0.01 ng/mL,定量限均为0.02 ng/mL,日内精密度及日间精密度均小于20％,相对回收率在98.38％～115.10％之间.检测到案件血液中地芬尼多和苯海拉明的浓度分别为4.02、3.78 μg/mL.本研究表明建立的血液中地芬尼多与苯海拉明的超声辅助离子液体-分散液液微萃取-液相色谱串联质谱法检测方法可行,具有环境友好、富集效率高、灵敏度高等优点,可应用于地芬尼多与苯海拉明相关案件的法医学鉴定.
A method for the determination of difenidol and diphenhydramine in blood samples utilizing ultrasonic-assisted ionic liquid dispersive liquid-liquid microextraction coupled with LC-MS/MS was established.l-butyl-3-methylimidazolium hexafluorophosphate([Bmim][PF6])was used as the extractant,and acetone was used as the dispersant.The samples were separated by a ZORBAX Eclipse Plus C18 RRHD column.Aqueous solution containing 0.1％formic acid and methanol was used as mobile phases.A gradient elution mode was employed with a flow rate of 0.2 mL/min,followed by electrospray ion source mode(ESI+)analysis in scheduled multiple reaction monitoring mode(MRM).The detection limits of difenidol and diphenhydramine in blood samples were 0.01 ng/mL,and the quantification limits were 0.02 ng/mL for both.The intraday and interday precisions(relative standard deviation,RSD)were both less than 20％,and the relative recovery rates ranged from 98.38％to 115.10％.The concentrations of difenidol and diphenhydramine in the blood of a fatal case were 4.02 μg/mL and 3.78 μg/mL,respectively.This study demonstrated the feasibility of using ultrasonic-assisted ionic liquid dispersive liquid-liquid microextraction combined with LC-MS/MS for the determination of difenidol and diphenhydramine in blood samples.The method has the advantages of environmentally friendly,high enrichment efficiency,and high sensitivity,making it suitable for forensic identification of difenidol and diphenhydramine.
师燕华;孙赟;郭月;管青林;王涛;胡萌;尉志文;贠克明;崔海燕
山西医科大学法医学院,法庭毒物分析公安部重点实验室,山西晋中 030600山西医科大学法医学院,法庭毒物分析公安部重点实验室,山西晋中 030600山西医科大学法医学院,法庭毒物分析公安部重点实验室,山西晋中 030600绍兴文理学院医学院,浙江绍兴 312000山西医科大学法医学院,法庭毒物分析公安部重点实验室,山西晋中 030600山西医科大学法医学院,法庭毒物分析公安部重点实验室,山西晋中 030600山西医科大学法医学院,法庭毒物分析公安部重点实验室,山西晋中 030600山西医科大学法医学院,法庭毒物分析公安部重点实验室,山西晋中 030600山西医科大学法医学院,法庭毒物分析公安部重点实验室,山西晋中 030600
社会科学
法医毒物分析超声辅助离子液体-分散液液微萃取液相色谱-串联质谱地芬尼多苯海拉明
forensic toxicological analysisultrasonic-assisted ionic liquid dispersive liquid-liquid microextraction(UAIL-DLLME)LC-MS/MSdifenidoldiphenhydramine
《刑事技术》 2026 (2)
142-148,7
国家重点研发计划(2017YFC0803504)国家青年科学基金项目(81601647)法医病理学公安部重点实验室2023年度开放课题(GAFYBL202304)山西省教育厅高校科技创新项目(2020L0191)
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