Hackett Jeffery, Elian Albert A
Forensic Toxicology Laboratory, Center for Forensic Sciences, 100 Elizabeth Blackwell Street, Syracuse, NY 13210, USA.
Forensic Sci Int. 2006 Mar 10;157(2-3):156-62. doi: 10.1016/j.forsciint.2005.03.019. Epub 2005 Jun 13.
The forensic toxicology community has recognized flunitrazepam and its metabolite (7-aminoflunitrazepam) as compounds of concern for several years. In this procedure, the analytes were extracted from whole blood and urine onto single mode solid phase cartridges (butyl) using nitrazepam as an internal standard. The columns were washed with distilled water and hexane. All three compounds were eluted from the sorbent using an ethyl acetate-methanol solvent mixture. After collection and evaporation of the solvent, the residue was dissolved in A, 0.1% (v/v) aqueous trifluoroacetic acid for HPLC-PDA analysis or B, ethyl acetate for derivatization with pentafluoropropionic anhydride (PFPA) for analysis by gas chromatography-mass spectrometry (selected ion monitoring, SIM). A limit of quantitation for this method using HPLC-PDA was found to be 5 and 1.0 ng mL(-1) by SIM.
多年来，法医毒理学界一直将氟硝西泮及其代谢物（7-氨基氟硝西泮）视为令人关注的化合物。在此方法中，以硝西泮作为内标，将分析物从全血和尿液中萃取到单模式固相柱（丁基柱）上。用蒸馏水和己烷冲洗柱子。使用乙酸乙酯 - 甲醇混合溶剂从吸附剂上洗脱所有三种化合物。收集并蒸发溶剂后，残留物溶解于A，用于高效液相色谱 - 光电二极管阵列检测（HPLC - PDA）分析的0.1%（v/v）三氟乙酸水溶液，或B，用于用五氟丙酸酐（PFPA）衍生化以进行气相色谱 - 质谱联用（选择离子监测，SIM）分析的乙酸乙酯。发现此方法使用HPLC - PDA时的定量限为5 ng mL(-1)，通过SIM为1.0 ng mL(-1)。
