MPFC-QuEChERS结合GC-MS/MS测定血液中γ-羟基丁酸  

Determination of γ-Hydroxybutyric Acid in Blood by MPFC-QuEChERS with GC-MS/MS

作　　者：李润康 李佳宜 张云峰[1] 董林沛 何洪源[2] 魏春明[1] LI Run-kang;LI Jia-yi;ZHANG Yun-feng;DONG Lin-pei;HE Hong-yuan;WEI Chun-ming(Institute of Forensic Science,Ministry of Public Security,Beijing 100038,China;School of Investigation,People’s Public Security University of China,Beijing 100038,China)

机构地区：[1]公安部物证鉴定中心,北京100038 [2]中国人民公安大学侦查学院,北京100038

出　　处：《分析测试学报》2022年第3期386-391,共6页Journal of Instrumental Analysis

基　　金：中央级公益性科研院所基本科研业务费项目(2020JB002)。

摘　　要：建立了一种快速多滤过型净化柱(MPFC)-QuEChERS结合气相色谱-串联质谱(GC-MS/MS)检测血液中γ-羟基丁酸(GHB)的新方法。通过考察样品前处理条件与仪器条件对检测结果的影响,确定了最优实验条件:0.1 mL血液样品中加入GHB-D;作为内标,以乙酸乙酯为萃取剂,上清液过MPFC-QuEChERS净化柱后挥干,经N,O-双三甲基硅烷基三氟乙酰胺(BSTFA)衍生化,在多反应监测(MRM)模式下分析。结果表明,血液中GHB在0~1 000 ng/mL质量浓度范围内线性关系良好,相关系数(r^(2))为0.995 1,检出限和定量下限分别为0.2、0.5 ng/mL,日间和日内相对标准偏差(RSD)均小于15%,回收率为80.1%~84.7%,基质效应为87.4%~94.4%。该方法由传统液液萃取法改进优化,稳定性好、灵敏度高,能够快速有效测定实际案件血液样品中的GHB含量。A new method was developed for the determination of γ-hydroxybutyric acid(GHB)in human blood by gas chromatography-tandem mass spectrometry(GC-MS/MS)with a kind of purification column(MPFC-QuEChERS).Effects of sample pretreatment conditions and analytical instrument conditions on the test results were investigated in the round,and the optimal experimental conditions were determined.First of all,GHB-D;was spiked into 0.1 mL blood sample as the internal standard,and then the analyte was extracted using ethyl acetate efficiently.After that,the supernatant was allowed to flow through the MPFC-QuEChERS purification column and evaporated to dryness.Finally, the dried residue was derivated with trifluoroacetamide(BSTFA)and analyzed in multi-reaction monitoring(MRM)mode.Experimental results showed that there were linear relationships for the spiked human blood samples in the range of 0-1 000 ng/mL(r^(2)> 0.995 1).The limits of detection(LOD)and limits of quantitation(LOQ)of the method were 0.2 ng/mL and 0.5 ng/mL,respectively.The inter-day relative standard deviations(RSD)and intra-day RSD were both less than15%.An extraction recovery of 80.1%-84.7%was obtained for the spiked human blood samples.The matrix effect ranged from 87.4%to 94.4%.The results indicated that the developed method was improved and optimized by traditional liquid-liquid extraction method,it could be applied to the rapid and effective determination of GHB in human blood samples of actual cases with its good stability and high sensitivity.

关 键 词：羟基丁酸 MPFC-QuEChERS 气相色谱-串联质谱 血液 

分 类 号：O657.63[理学—分析化学] S859.81[理学—化学]