Bogusz M J, Maier R D, Krüger K D, Früchtnicht W
Institute of Forensic Medicine, Aachen University of Technology, Germany.
J Chromatogr B Biomed Sci Appl. 1998 Aug 25;713(2):361-9. doi: 10.1016/s0378-4347(98)00207-2.
A selective assay of flunitrazepam (F) and its metabolites 7-aminoflunitrazepam (7-AF), N-desmethylflunitrazepam (N-DF) and 3-hydroxyflunitrazepam (3-OHF) with liquid chromatography-atmospheric pressure chemical ionization mass spectrometry (LC-APCI-MS, positive ions) is described. The drugs were isolated from serum, blood or urine using a solid-phase extraction procedure previously applied to various drugs of abuse. F-d3 and 7-AF-d3 were used as internal standards. The drugs were separated on ODS column in acetonitrile-50 mM ammonium formate buffer, pH 3.0 (45:55, v/v). After analysis of mass spectra taken in full scan mode, a selected-ion monitoring detection was applied with following ions: m/z 284 (7-AF and F), 287 (7-AF-d3 and F-d3), 314 (F), 300 (N-DF and 3-OHF), 317 (F-d3), 330 (3-OHF). The limits of detection were: 0.2 microg/l for F and 7-AF, 1 microg/l for N-DF and 3-OHF. The method was linear in the range 1-500 microg/l, the recoveries ranged from 92 to 99%. The method was applied for determination of F and metabolites in clinical and forensic samples. LC-APCI-MS seems to be a method of choice for these compounds.
描述了一种采用液相色谱 - 大气压化学电离质谱法（LC - APCI - MS，正离子模式）对氟硝西泮（F）及其代谢物7 - 氨基氟硝西泮（7 - AF）、N - 去甲基氟硝西泮（N - DF）和3 - 羟基氟硝西泮（3 - OHF）进行选择性分析的方法。使用先前应用于各种滥用药物的固相萃取程序从血清、血液或尿液中分离出这些药物。F - d3和7 - AF - d3用作内标。药物在ODS柱上，以乙腈 - 50 mM甲酸铵缓冲液（pH 3.0，45:55，v/v）进行分离。在全扫描模式下采集质谱图进行分析后，采用选择离子监测检测，监测以下离子：m/z 284（7 - AF和F）、287（7 - AF - d3和F - d3）、314（F）、300（N - DF和3 - OHF）、317（F - d3）、330（3 - OHF）。检测限为：F和7 - AF为0.2 μg/l，N - DF和3 - OHF为1 μg/l。该方法在1 - 500 μg/l范围内呈线性，回收率在92%至99%之间。该方法应用于临床和法医样本中F及其代谢物的测定。LC - APCI - MS似乎是分析这些化合物的首选方法。
