Jagerdeo Eshwar, Montgomery Madeline A, LeBeau Marc A
Federal Bureau of Investigation Laboratory, 2501 Investigation Parkway, Quantico, VA 22135, USA
Federal Bureau of Investigation Laboratory, 2501 Investigation Parkway, Quantico, VA 22135, USA.
J Anal Toxicol. 2015 Mar;39(2):83-8. doi: 10.1093/jat/bku130. Epub 2014 Nov 28.
The abuse of gamma-hydroxybutyric acid (GHB) and its suspicion in cases of suspected drug-facilitated sexual assault is of keen interest to forensic toxicology laboratories. This paper reports an extraction, separation and detection procedure for GHB in hair utilizing a combination of liquid-liquid extraction and solid-phase extraction using ethyl acetate and Oasis Max(®) cartridge, respectively, after the hair sample was digested. Analysis was by LC-MS-MS using a gradient separation on an Acclaim(®) Trinity(TM) P1 column performing three multiple-reaction monitoring (MRM) transitions each for GHB and its internal standard. The procedure was validated over a range from 0.4 to 50 ng/mg with estimated limit of detection (LOD) of 0.33 and an administratively set limit of quantitation (LOQ) of 1.2 ng/mg. Twenty hair specimens collected from individuals with no known exposure to GHB were analyzed for matrix interferences and to establish initial background levels of GHB. A wide range of endogenous GHB levels were observed in these samples (from less than the LOQ to 4.4 ng/mg). The results suggest the need for additional studies to better establish the full range of endogenous GHB levels in hair and that extreme caution is required in interpreting GHB findings in hair samples.
γ-羟基丁酸（GHB）的滥用及其在疑似药物辅助性性侵案件中的嫌疑引起了法医毒理学实验室的密切关注。本文报道了一种毛发中GHB的提取、分离和检测方法，该方法在毛发样品消化后，分别使用乙酸乙酯和Oasis Max® 柱进行液-液萃取和固相萃取相结合的操作。分析采用LC-MS-MS，在Acclaim® Trinity™ P1柱上进行梯度分离，对GHB及其内标物各自进行三次多反应监测（MRM）转换。该方法在0.4至50 ng/mg范围内得到验证，估计检测限（LOD）为0.33，行政设定的定量限（LOQ）为1.2 ng/mg。对20份来自无已知GHB暴露个体的毛发样本进行分析，以检测基质干扰并确定GHB的初始背景水平。在这些样本中观察到了广泛的内源性GHB水平范围（从低于LOQ到4.4 ng/mg）。结果表明需要进行更多研究以更好地确定毛发中内源性GHB水平的完整范围，并且在解释毛发样本中的GHB检测结果时需要格外谨慎。
