ICP-MS法测定多西他赛原料药中的10种金属元素杂质

Determination of Ten Metal Elemental Impurities in Docetaxel with Inductively Coupled Plasma Mass Spectrometry

目的:建立测定多西他赛原料药中镉、铅、砷、汞等10种金属元素杂质的电感耦合等离子体质谱法。方法:用锗、铟、铋作为内标元素校正基体干扰和漂移,微波消解法处理样品,并对三个不同厂家的多西他赛原料药进行检测。结果:在优化的实验条件下,镉、铅、砷、汞、钴、钒、镍在1.0~50.0μg/L范围内呈良好的线性关系,锂、锑、铜在10.0~500.0μg/L范围内呈良好的线性关系,标准曲线相关系数(r)均≥0.9993;各元素的平均回收率均在90%~110%范围内,RSD均小于4%;三个不同厂家的多西他赛原料药中各元素杂质均在允许限度范围内。结论:ICP-MS法灵敏度高、准确度和精密度良好,适用于多西他赛原料药中金属元素杂质的测定。

Objective To establish an inductively coupled plasma mass spectrometry method, for the determination of ten kinds of metal element impurities in docetaxel, such as cadmium, lead, arsenic and mercury, etc. Methods The germanium, indium and bismuth are used as the internal standard elements to calibrate the matrix interference and drift, microwave digestion method is used to process samples, and test three batches of docetaxel from different companies using the established method. Results Under the optimized experimental conditions, the linearity of regression equations are good, when the concentrations of these elements including cadmium, lead, arsenic, mercury, cobalt, vanadium, nickel are within 1.0-50.0μg/L, and the concentrations of other elements including lithium, antimony, copper are within 10.0-500.0μg/L. The standard curve correlation coefficient （r） are all equal or greater than 0.9993. The average recovery rate of each element are within 90 %-110 %, the RSD are all less than 4 %, and each metal element impurities of three batches of docetaxel from different companies are within the permissible limits. Conclusion The established ICP-MS method is of high sensitivity, good accuracy and precision, and is suitable for the determination of metal element impurities in docetaxel.