Yoshida M, Watabiki T, Tokiyasu T, Saito I, Ishida N
Department of Legal Medicine, Kansai Medical University, Moriguchi, Japan.
Nihon Hoigaku Zasshi. 1993 Jun;47(3):220-6.
Thermospray liquid chromatography mass spectrometric method is described for the determination of the benzodiazepines (Nitrazepam, Estazolam, Bromazepam, Flunitrazepam). Reversed-phase liquid chromatography was performed using a 15 cm Shim-pack CLC-ODS (Shimadzu) column, with acetonitrile-water (40:60) + 0.1 M ammonium acetate as mobile phase, at a flow rate of 1.0 ml/min. The temperature of the vaporizer, block and TH of the source block were 166, 270 and 275 degrees C, respectively. Positive ion thermospray mass spectra by thermospray ionization (TSP ionization) mode or thermospray on filament ionization (filament-on ionization) mode were obtained. Formation of the MH+ ion was observed as a base peak under TSP ionization and filament-on ionization conditions and fragment ions were very few. On both ionization mode, peaks representing nitrazepam as MH+ at m/z 282 at a retention time (R.T.) of 6.4 min, from estazolam as MH+ at m/z 295 at an R.T. of 6.4 min, from bromazepam as MH+ at m/z 316 at an R.T. of 4.5 min and from flunitrazepam as MH+ at m/z 314 at an R.T. of 8.8 min. The detection limit for all the benzodiazepines under investigation was less than 0.5 ng (S/N = 9.4 +/- 4.6) using selected ion monitoring.
本文描述了热喷雾液相色谱质谱法用于测定苯二氮䓬类药物（硝西泮、艾司唑仑、溴西泮、氟硝西泮）。采用15 cm Shim-pack CLC-ODS（岛津）柱进行反相液相色谱分析，以乙腈-水（40:60）+ 0.1 M醋酸铵为流动相，流速为1.0 ml/min。蒸发器、加热块和源加热块的温度分别为166、270和275℃。通过热喷雾电离（TSP电离）模式或热喷雾灯丝电离（灯丝开启电离）模式获得正离子热喷雾质谱。在TSP电离和灯丝开启电离条件下，观察到MH⁺离子的形成作为基峰，且碎片离子很少。在两种电离模式下，硝西泮以m/z 282的MH⁺形式在保留时间（R.T.）6.4分钟出现峰，艾司唑仑以m/z 295的MH⁺形式在R.T. 6.4分钟出现峰，溴西泮以m/z 316的MH⁺形式在R.T. 4.5分钟出现峰，氟硝西泮以m/z 314的MH⁺形式在R.T. 8.8分钟出现峰。使用选择离子监测，所有所研究的苯二氮䓬类药物的检测限均小于0.5 ng（S/N = 9.4 ± 4.6）。
