LeBeau M A, Montgomery M A, Wagner J R, Miller M L
Chemistry Unit, FBI Laboratory, Federal Bureau of Investigation, Washington, DC 20535, USA.
J Forensic Sci. 2000 Sep;45(5):1133-41.
A rapid and sensitive liquid chromatography/electrospray ionization mass spectrometry (LC/MS) procedure has been developed for the analysis of biofluids containing flunitrazepam and its metabolites. Specimens were spiked with deuterated analogs of the analytes. Urine specimens were enzymatically hydrolyzed and blood specimens were untreated. Extractions were carried out using CleanScreen DAU SPE cartridges. The drugs were separated on a C18 column using a methanol-water-ammonium hydroxide (60:40: 0.03 v/v) mobile phase. After determination of base peaks using full scan mass spectrometry, the mass spectrometry method was optimized to operate in selected-ion monitoring (SIM) mode for the base peak of each analyte. Positive findings were confirmed by LC/MS/MS using the same mobile phase and column. This analytical procedure allows for the detection of low levels of flunitrazepam and metabolites in biofluids. It is useful for ascertaining the role of flunitrazepam in cases of drug-facilitated sexual assault.
已开发出一种快速灵敏的液相色谱/电喷雾电离质谱（LC/MS）方法，用于分析含有氟硝西泮及其代谢物的生物流体。样本中加入了分析物的氘代类似物。尿液样本进行酶解，血液样本不做处理。使用CleanScreen DAU固相萃取柱进行萃取。药物在C18柱上分离，流动相为甲醇-水-氢氧化铵（60:40:0.03 v/v）。通过全扫描质谱法测定基峰后，将质谱方法优化为对每种分析物的基峰以选择离子监测（SIM）模式运行。使用相同的流动相和色谱柱，通过LC/MS/MS确认阳性结果。该分析方法可检测生物流体中低水平的氟硝西泮及其代谢物。它有助于确定氟硝西泮在药物辅助性性侵案件中的作用。
