Liu Wei, Shen Min, Xiang Ping, Bu Jun, Wu He-Jian
Institute of Forensic Sciences, Ministry of Justice, P.R. China, Shanghai 200063, China.
Fa Yi Xue Za Zhi. 2007 Apr;23(2):120-2, 129.
To establish an analytical method for the determination of GHB in beverages using GC/MS and LC/MS/MS.
After beverage samples with GHB-d6 as the internal standard were extracted with ethyl acetate, then the extracts were derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA), at last the derivateized extracts analyzed by gas chromatography- mass spectrometry. After beverage samples with GHB-d6 as the internal standard were diluted by mobile phase then directly analyzed by LC/MS/MS. Results The limit of detection was 0.2 microg/mL and both relative standard deviations for between-day and within-day assays were < 8.54% in GC/MS. The limit of detection was 2 microg/mL and both relative standard deviations for between-day and within-day assays were <8.62% in LC/MS/MS. Conclusion These methods of qualitative and quantitative analysis were found to be sensitive, accurate, rapid and suitable for the forensic toxicology to test of GHB in real cases.
建立一种使用气相色谱/质谱联用仪(GC/MS)和液相色谱/串联质谱仪(LC/MS/MS)测定饮料中γ-羟基丁酸(GHB)的分析方法。
以氘代γ-羟基丁酸(GHB-d6)为内标物的饮料样品用乙酸乙酯萃取后,提取物用N,O-双(三甲基硅基)三氟乙酰胺(BSTFA)进行衍生化,最后衍生化提取物通过气相色谱-质谱联用仪进行分析。以GHB-d6为内标物的饮料样品用流动相稀释后直接通过LC/MS/MS进行分析。结果气相色谱/质谱联用仪检测限为0.2微克/毫升,日间和日内测定的相对标准偏差均<8.54%。液相色谱/串联质谱仪检测限为2微克/毫升,日间和日内测定的相对标准偏差均<8.62%。结论这些定性和定量分析方法灵敏、准确、快速,适用于法医毒理学实际案件中GHB的检测。