Development of rapid and sensitive methods for the forensic analysis of xenobiotic substances in hair

建立了一种用于13种镇静催眠药分析的新的样品前处理方法。用3.0M磷酸铵微粉萃取后，用QExactive混合质谱计鉴定分析物。样本量要求减少到5毫克。最低定量限(LLOQ)为1pg/mg的溴唑仑、安定、N-脱甲基安定、艾司唑仑、氟硝西仑、硝基安定、三唑仑、雷美替隆和唑吡坦，4pg/mg的阿普唑仑、N-脱甲基氟安定、依地唑仑和佐匹克隆。所有分析物的重复分析的准确度和精密度在三种浓度下都符合FDA的指南。开发的方法被应用于四名睡眠障碍患者的头发样本。与以前的方法相比，本方法需要较少的样品，在较短的分析时间内完成。这些方法的改进将有助于从DFSA受害者的头发样本中检测服用镇静催眠药的情况。

We established a new sample preparation method for the analysis of 13 sedative-hypnotics. Following micropulverized extraction with 3.0 M ammonium phosphate, a QExactive hybrid mass spectrometer was used to identify the analytes. The sample size requirement was reduced to 5 mg. The lower limits of quantification (LLOQ) were 1 pg/mg for brotizolam, diazepam, N-desmethyldiazepam, estazolam, flunitrazepam, nitrazepam, triazolam, ramelteon and zolpidem, and 4 pg/mg for alprazolam, N-desmethylfludiazepam, etizolam and zopiclone. Accuracy and precision of the repeated analyses for all the analytes met FDA guidelines at three concentrations. The developed method was applied to hair samples from four patients with sleep disorders. Compared with earlier methods, the present method requires a smaller amount of sample and is complete within a shorter analytical time. These method improvements will be helpful for detecting administration of sedative-hypnotics from hair samples of victims of DFSA.