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.
作者
李润康
李佳宜
张云峰
董林沛
何洪源
魏春明
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)
出处
《分析测试学报》
CAS
CSCD
北大核心
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)。
