吡哌酸片中元素杂质的电感耦合等离子体质谱法测定

Determination of the Elemental Impurities in Pipemidic Acid Tablets by ICP-MS

目的:建立吡哌酸片中元素杂质的电感耦合等离子体质谱测定方法。方法:采用微波消解提取元素杂质,电感耦合等离子体质谱仪(ICP-MS)检测吡哌酸片中的21种元素杂质。结果:汞在0～10 ng·ml^(-1)范围内线性关系良好,其他20种目标元素在0～100 ng·ml^(-1)范围内线性关系良好,r均>0.999 0。平均回收率为80%～120%,RSD为0.26%～7.75%(n=9)。采用本法检测了44批次市售吡哌酸片中的元素杂质,结果均未超过规定限度。结论:该方法操作简便,分析速度快,灵敏度高,适用于吡哌酸片中元素杂质的测定。

Objective: To establish a determination method for the elemental impurities in pipemidic acid tablets by inductively coupled plasma mass spectrometry (ICP-MS). Methods: Microwave digestion was used to extract the elemental impurities,and ICPMS was used to detect 21 elemental impurities in pipemidic acid tablets. Results: Mercury had a good linear relationship within the range of 0-10 ng·ml-1,all the other 20 target elements had good linear relationships within the range of 0-100 ng·ml-1,and r was greater than 0.999 0. The sample addition recovery was 80%-120% and the RSD was 0.26%-7.75% (n = 9). The elemental impurities in 44 batches of commercially available pipemidic acid tablets were tested and all the results didn’t exceed the limits. Conclusion: The method is simple,rapid and accurate,and can be used for the quality control of trace elements and heavy metals in pipemidic acid tablets.