Development of automatic extraction-analysis system for thermospray mass spectrometer.

我们展示了一个自动的，在线提取分析测定苯二氮卓类药物（溴西泮，艾司唑仑和三唑仑）的柱切换系统的三个柱，使用热喷雾液相色谱-质谱仪和光电二极管阵列检测器。血清中的苯二氮卓类药物用凝胶柱（ASAHIPAKGS-310 HC 18，4.6mmID * 250 mmL）和移动的流动相1（含0.1NNaClO_4的40%CH_3CN，流速0.5ml/min）分离，然后捕集到第二柱（CAPCELL PAKC 18，4.6mmID * 35 mmL）上。用移动的流动相2（蒸馏水，流速1.5ml/min，5 min）洗柱后，用第三根色谱柱（STR ODS-2，4.6mm ID* 250 mm L）和移动的流动相3（50%CH_3，<3CN>含50 mM CH_3COONH_4和0.05%CH_3COOH，流速1.0ml/min）鉴别每种药物。采用热喷雾质谱仪QP 1000 EX和光电二极管阵列检测器SPD-M10 AVP对苯二氮卓类药物进行检测，离子源模块的蒸发器、模块和尖端加热器的温度分别设置为144、305和315 ℃。溴西泮、艾司唑仑和三唑仑的峰分别为4.8、6.3和7.1 min。水溶液中药物的回收率分别为90.9%、97.2%和90.9%。三种药物的重复性变异系数分别为1.25、0.33和0.54%。溴西泮、艾司唑仑和三唑仑的基峰分别为m/z316、295和343。

We demonstrate an automatic, on-line extraction-analysis assay for benzodiazepines (bromazepam, estazolam and triazolam) by the column-switching system for three columns using thermospray liquid chromatograph-mass spectrometer and photodiode array detector. The benzodiazepines in serum were separated from the serum contents using a gel column (ASAHIPAK GS-310H C18,4.6mm ID*250mm L) and the mobile phase 1 (40% CH_3CN containing 0.1 N NaCIO_4 at a flow rate of 0.5ml/min), and then trapped to the second column (CAPCELL PAK C18,4.6mm ID*35mm L). Following the column-wash with the mobile phase 2 (distillled water at 1.5ml/min, for 5min), each drug was identified using the third column (STR ODS-2,4.6mm ID*250mm L) and the mobile phase 3 (50% CH_<3CN> containing 50 mM CH_3COONH_4 and 0.05% CH_3COOH,at 1.0ml/min). The benzodiazepines were detected thermospray mass spectrometer QP1000EX and photodiode array detector SPD-M10AVP.The temperature of the vaporizer, block and tip heater of the ion source block were set at 144,305 and 315 ﾟC,respectively. Peaks of bromazepam, estazolam and triazolam were represented 4.8,6.3 and 7.1 min, respectively. The recovery rates of the drugs in aqueous solution were 90.9,97.2 and 90.9%, respectively. The coefficients of variance for reproducibility of the drugs were 1.25,0.33 and 0.54%, respectively. When thermospray ionization was used, MH^+ ions of m/z 316,295 and 343 were obtained as base peak for bromazepam, estazolam and triazolam, respectively.