尿液、血液中γ-羟丁酸的气质联用法分析

目的为尿液、血液中γ-羟丁酸(gamma-hydroxybutyricacid,GHB),γ-羟丁酸内酯(gamma-butyrolactone,GBL)和1,4-丁二醇(1,4-butanediol,1,4-BD)的鉴定提供方法和依据。方法100μl尿液或血液以GHBd6为内标,经乙酸乙酯提取、BSTFA衍生化后,用GC／MS法分析。结果测尿液中内源性GHB的线性范围是20-800ng／ml,R2=0.9995,最低检出限为10ng／ml(S／N≥3);测尿液、血液中外源性GHB的线性范围为5-60μg／ml,R2分别为0.9999和0.9928。相对回收率为99％-104％。以所建方法测定了健康志愿者尿液中内源性GHB含量,并考察了健康受试者外源性GHB的代谢情况。结论所建方法准确、便捷、省时、选择性好,适用于法医毒物学鉴定。

Determination of Gamma-hydroxybutyric acid in urine and blood by GC-MS

Objective To provide methods for detection of gamma-hydroxybutyric acid (GHB), gamma-butyrolactone (GBL) and 1,4-butanediol (1,4-BD). Methods 100μl urine or blood sample was extracted with ethyl acetate. The extracts were derived with BSTFA, and analyzed by gas chromatographymass spectrometry using GHB-d6 as the internal standard. Results Linear limits of endogenous GHB detected in urine ranged from 20ng/ml to 800ng/ml (R2=0.9995). Limit of detection was 10ng/ml (S/N≥3). Linear limits of exogenous GHB in urine and blood were from 5μg/ml to 60μg/ml (R2=0.9999 and 0.9928 respectively). The relative recoveries were calculated from 99% to 104%. The concentrations of endogenous GHB in urine specimens from GHB-free subjects were detected, and dynamic GHB levels in the blood and urine of the healthy volunteers were evaluated by using the methods. Conclusion The methods are sensitive, simple, rapid, and suitable for determination of GHB in human blood and urine for forensic toxicological analysis.