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作 者:刘伟[1] 沈敏[1] 向平[1] 卜俊[1] 吴何坚[1]
机构地区:[1]司法部司法鉴定科学技术研究所,上海200063
出 处:《法医学杂志》2007年第2期120-122,129,共4页Journal of Forensic Medicine
基 金:上海市科委司法鉴定技术标准项目(2003DIB7J055-3)
摘 要:目的建立饮料中γ-羟基丁酸(GHB)的分析方法。方法检材以GHB-d6为内标,加入酸性氯化铵饱和溶液调节pH值<4,用乙酸乙酯提取、离心后取有机层,水浴下吹干,经BSTFA衍生化后,用气相色谱/质谱联用仪测定。检材以GHB-d6为内标,经流动相稀释、离心后,吸取上清液用液相色谱-串联质谱仪测定。结果GC/MS测定饮料中GHB的检出限为0.2μg/mL,日内精密度和日间精密度小于8.54%;LC/MS/MS测定饮料中GHB的检出限为2μg/mL,日内精密度和日间精密度小于8.62%。结论饮料中GHB进行定性定量分析。方法灵敏、准确、快速,适用于法庭毒物分析中饮料中GHB的检测。Objective To establish an analytical method for the determination of GHB in beverages using GC/MS and LC/MS/MS. Methods 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 0.2μg/mL and both relative standard deviations for between-clay and within-clay assays were 〈 8.54% in GC/MS. The limit of detection was 2μg/mL and both relative standard deviations for between-clay and within-clay 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.
关 键 词:γ-羟基丁酸(GHB) 饮料 气相色谱/质谱联用法 液相色谱-串联质谱法 法庭毒物分析
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