采用液相色谱联用电化学反应装置对药物氧化加速降解过程在线监测

On-line Hyphenated Chromatographic Electrochemical Instrument for Improving Accelerated Oxidation Degradation Test

采用液相色谱在线联用电化学反应装置(ECI)对药物氧化加速降解试验进行改进。以叔丁基对苯二酚为模型药物,对高压六通切换阀的切换时间、库仑电化学检测器的操作电压、输液泵流速进行筛选,并通过HPLC-UV检测原型和氧化产物的含量变化,确定最优的氧化破坏实验条件,最后采用高效液相色谱-二级阵列管检测法对氧化产物进行初步鉴定。结果表明,采用ECI系统进行药物氧化降解试验的最优条件为:六通阀切换时间为30 s,库仑检测器氧化电压为150 m V,输液泵流速为0.2 m L/min。氧化产物经初步鉴定为叔丁基苯醌(TQ)。此装置及其方法可有效缩短时间和简化步骤,实现氧化加速降解试验从样品处理到分离检测的自动化和在线化。

In order to improve the accelerated oxidation degradation test,the method by using an on-line hyphenated chromatographic electrochemical instrument（ ECI） was established. Tert butyl hydroquinone（ TBHQ） was selected as modal drug to optimize several conditions factors of ECI including applied potential of Columba electrochemical detector,stretch time of high voltage switching six-way valve and flow rate. The optimized conditions were obtained after all above investigations were finished. The oxidant of TBHQ was identified by the high preference liquid chromatography-diode array detector. The optimized conditions including applied potential of Columba electrochemical detector,stretch time of high voltage switching six-way valve and flow rate were 150 m V,30 s and 0. 2 m L / min,respectively. The oxidant of TBHQ was preliminarily identified as tert butyl quinine（ TQ）. The method based ECI was on-lined and automated and will be very useful in improving accelerated oxidation degradation test.