Stout Phillip A, Simons Kelsie D, Kerrigan Sarah
Forensic Science Program, College of Criminal Justice, Sam Houston State University, Box 2525, 1003 Bowers Blvd, Huntsville, TX 77341, USA.
J Forensic Sci. 2010 Mar 1;55(2):531-7. doi: 10.1111/j.1556-4029.2009.01304.x. Epub 2010 Feb 5.
A method capable of quantifying endogenous concentrations of gamma-hydroxybutyrate (GHB) in human head hair was developed and validated using liquid chromatography/mass spectrometry/mass spectrometry (LC/MS/MS). Hair was digested under alkaline conditions, and GHB was isolated using liquid-liquid extraction. LC/MS/MS was performed using atmospheric pressure chemical ionization in the negative mode, multiple reaction monitoring, and deuterated internal standard (GHB-D(6)). Linearity was observed between 0.1 and 100 ng/mg GHB (R(2) = 1.000). The limits of detection and quantitation in human hair were 0.2 and 0.4 ng/mg, respectively. Accuracy at 2 ng/mg and 10 ng/mg was determined to be 97% and 94%, and intra-assay CVs at these concentrations were 5.2% and 7.4% (n = 4). Beta-hydroxybutyrate (BHB), alpha-hydroxybutyrate, gamma-butyrolactone, and 1,4-butanediol did not produce an interference, and there was negligible ion suppression or enhancement from the matrix.
开发了一种能够使用液相色谱/质谱/质谱（LC/MS/MS）对人头发中γ-羟基丁酸（GHB）的内源性浓度进行定量的方法，并进行了验证。头发在碱性条件下消化，使用液液萃取分离GHB。LC/MS/MS采用大气压化学电离负模式、多反应监测和氘代内标（GHB-D(6)）进行。在0.1至100 ng/mg GHB之间观察到线性关系（R(2)=1.000）。人头发中的检测限和定量限分别为0.2和0.4 ng/mg。2 ng/mg和10 ng/mg时的准确度分别为97%和94%，这些浓度下的批内变异系数分别为5.2%和7.4%（n = 4）。β-羟基丁酸（BHB）、α-羟基丁酸、γ-丁内酯和1,4-丁二醇未产生干扰，基质的离子抑制或增强可忽略不计。
