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

建立了一种新的样品前处理方法，用于13种镇静催眠药的分析。用3.0 M磷酸铵进行微粉碎提取后，使用QExactive混合质谱仪鉴定分析物。样本量要求降至5 mg。溴替唑仑、地西泮、N-去甲基地西泮、艾司唑仑、氟硝西泮、硝西泮、三唑仑、雷美替酮和唑吡坦的定量下限（LLOQ）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（LLOQ）为4 pg/mg。在三种浓度下，所有分析物重复分析的准确度和精密度均符合FDA指南。所开发的方法被应用于从四个睡眠障碍患者的头发样本。与以前的方法相比，本方法所需样品量少，分析时间短。这些方法的改进将有助于从DFSA受害者的头发样品中检测镇静催眠药。

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.