薄层色谱扫描和气相色谱-质谱法快速检测血中2,4-滴丁酯  

Rapid detection of 2,4-dbutylate in blood by TLCS and GC-MS

作　　者：李鹏[1] 贾雪峰[2] 韩胜[1] 贠克明[1] 

机构地区：[1]山西医科大学法医学院,太原030001 [2]北京市公安局西城分局法医检验检定所,北京100032

出　　处：《中国卫生检验杂志》2008年第2期204-207,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的：建立血中2,4-滴丁酯的薄层色谱扫描（TLCS）和气相色谱-质谱（GC-MS）快速定性定量检测方法。方法：样品经提取,点于GF254板上,展开后进行TLC扫描,比移值结合薄层扫描光谱图定性检测血液中2,4-滴丁酯。样品中加入内标邻苯二甲酸二异丁酯,提取后用GC-MS测定,特征离子片段定性,选择离子模式定量检测血液中2,4-滴丁酯。结果：TLCS分析,2,4-滴丁酯分别以环己烷-丙酮（4：1）和环己烷-氯仿（5：1）为展开剂,比移值（R f）分别为0.71及0.29,薄层扫描最大吸收波长为232 nm和285 nm。GC-MS分析,2,4-滴丁酯特征片段为57、185和276,选择离子模式定量检测线性范围为0.25～100.0μg/ml,最低检出限为0.1μg/ml（S/N=3）。结论：建立的血中2,4-滴丁酯的提取、TLCS和GC-MS检测方法可应用于2,4-滴丁酯中毒的快速检验诊断和中毒死亡的法医学鉴定。Objective：To establish a rapid analysis method for the quantitative and quanlitative detection of 2,4-Dbutylate in blood by a TLCS and GC-MS.Methods：The specimens were extracted with trichloromethane.GF254 was used as the stationary phase and cyclohexane：acetone（4：1）or cyclohexane：chloroform（5：1） as the mobile phase in the TLCS analysis.According to the Rf and the TLC scaning spectrum,the 2,4-Dbutylate in blood was identified.DB-5MS quartz capillary column,Electron Impact source（EI）,splitless mode were disposed in GC-MS,and diisobutyl phthalate was used as the internal standard.The qualitative analysis of 2,4-Dbutylate in blood was executed by the selected ion monitoring.Results：The Rfs of 2,4-Dbutylate were 0.71 and 0.29 respectively by the two different mobile phases.The absorption maximum wavelengths of 2,4-Dbutylate by the TLCS was 232 nm and 285 nm.The selected ion of 2,4-Dbutylate was 57,185,276 in SIM.The linear range of quantitative analysis was 0.25~100.0 μg/ml.The detected limit was 0.1 μg/ml（S/N=3）.Conclusion：The TLCS and GC-MS analysis can be used for the rapid diagnosis of 2,4-Dbutylate poisoning and forensic identification of 2,4-Dbutylate poisoning death.

关 键 词：2 4-滴丁酯 中毒 薄层色谱 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学]