目的:建立基于四极杆碰撞/反应池(DRC)技术的电感耦合等离子体质谱(ICP-MS)法测定硫酸氢氯吡格雷中镉(Cd)、铅(Pb)、砷(As)、汞(Hg)、钴(Co)、钒(V)和镍(Ni)7种元素杂质的分析方法。方法:采用5%硝酸溶液超声溶解样品后,用密闭超高压微波消解技术对样品进行了物质消解,同时应用四极杆碰撞/反应池(DRC)技术消除多原子离子对待测元素的干扰,并选用铟(In)、锗(Ge)、铋(Bi)、钪(Sc)元素为内标混合液校正基体干扰和漂移。结果:7种元素杂质的检测下限为0.001~0.013 μg·L-1,7种元素杂质的RSD均小于4.0%,通过添加标准回收试验,7种元素杂质的回收率在92%~110%范围内。3批样品中7种元素杂质检测结果均符合要求。结论:该法简便、快速、灵敏,可准确测定硫酸氢氯吡格雷(Ⅰ型)中7种元素杂质的残留量。
Objective: To develop a Dynamic Reaction CellTM(DRC) technology inductively coupled plasma mass spectrometry(ICP-MS) for the determination of cadmium(Cd), plumbum(Pb), arsenic(As), hydrargyrum(Hg), cobaltum(Co), vanadium(V) and Nickel(Ni) in clopidogrel sulfate. Methods: Samples were dissolved in 5% HNO3 by ultrasound, and then were decomposed in the ultra high pressure microwave digestion instrument, followed by dilution with ultrapure water. The above 7 heavy metal elements in the solution were then analyzed directly by ICP-MS. The use of ORS could eliminate the interference of polyatomic ions dramatically. In, Ge, Bi and Sc were used to correct the matrix interference and drift. Results: The detection limits of the 7 elemental impurities were in the ranges of 0.001-0.013 μg·L-1, the relative standard deviation of the 7 elemental impurities were less than 4.0% , and the recoveriesof the 7 elemental impurities were 92%-110% by adding standard recovery experiments. The test results of 7 elements in 3 batches of samples met the requirements. Conclusion: This method is rapid, simple and applicable for the analysis of trace elemental impurities in clopidogrel sulfate.
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