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

建立了一种分析13种镇静催眠药的新样品制备方法。用3.0 M磷酸铵进行微粉萃取后，采用QExactive混合质谱仪对分析物进行鉴定。样本量要求减少到5毫克。溴替唑仑、地西泮、n -去甲基地西泮、依司唑仑、氟硝西泮、硝西泮、三唑仑、拉美替恩和唑吡坦的定量下限为1 pg/mg，阿普唑仑、n -去甲基氟地西泮、依替唑仑和佐匹克隆的定量下限为4 pg/mg。在三种浓度下，所有分析物的重复分析的准确性和精密度均符合FDA指南。该方法应用于4名睡眠障碍患者的头发样本。与以前的方法相比，本方法所需的样品量更少，分析时间更短。这些方法的改进将有助于从DFSA受害者的头发样本中检测镇静催眠药物的施用。

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.