微波消解-电感耦合等离子体质谱法同时测定蒙脱石散中36种无机元素杂质含量  

Determination of 36 Inorganic Elemental Impurities in Montmorillonite Powder by Microwave Digestion - ICP - MS

作　　者：熊欢 陈萱 朱琼 XIONG Huan;CHEN Xuan;ZHU Qiong(Taizhou Institute for Drug Control,Taizhou,Jiangsu,China 225300;Nanjing University of Chinese Medicine Hanlin College,Taizhou,Jiangsu,China 225300)

机构地区：[1]江苏省泰州市药品检验院,江苏泰州225300 [2]南京中医药大学翰林学院,江苏泰州225300

出　　处：《中国药业》2025年第9期75-79,共5页China Pharmaceuticals

基　　金：江苏省市场监督管理局科技计划项目[KJ2023074]。

摘　　要：目的建立同时测定蒙脱石散中36种无机元素杂质含量的电感耦合等离子体质谱(ICP-MS)法。方法采用微波消解法处理样品,测试模式为碰撞池模式(KED),等离子体输出功率为1550 W,采样深度为8 mm,最大载流量为1.045 L/min,冷却气流量为14 L/min,辅助气流量为0.9 L/min,蠕动泵转速为40 r/min,进样系统为耐酸系统,手动进样,重复测定3次。结果36种无机元素杂质分别在各自质量浓度范围内与响应值比值的线性关系良好(r>0.995,n=6);重复性试验的RSD为3.13%~15.06%(n=6),日间精密度试验的RSD为1.85%~11.56%;平均回收率为77.17%~102.85%,RSD为1.67%~15.16%(n=9)。5批样品中36种无机元素杂质含量均低于限度值和控制阈值。结论该方法灵敏度高、准确性好,可用于蒙脱石散中36种无机元素杂质的含量测定。Objective To establish an inductively coupled plasma-mass spectrometry(ICP-MS)method for the simultaneously determination of 36 inorganic element impurities in Montmorillonite Powder.Methods Microwave digestion method was used to process the sample,the testing mode was kinetic energy discrimination(KED),the plasma output power was 1550 W,the sampling depth was 8 mm,and the maximum current carrying capacity was 1.045 L/min,the flow rate of cooling air was 14 L/min,the flow rate of auxiliary air was 0.9 L/min,the speed of peristaltic pump was 40 r/min,the injection system was an acid resistant system,with manual injection and repeated measurements three times.Results The 36 inorganic element impurities had a good linear relationship(r>0.995,n=6).The RSD of the repeatability test was in the range of 3.13%-15.06%(n=6),and the RSD of the intra-day precision test was in the range of 1.85%-11.56%.The average recoveries of 36 inorganic element impurities were in the range of 77.17%-102.85%,with RSDs of 1.67%-15.16%(n=9).The impurity content of 36 inorganic element impurities in five batches of samples was lower than the limit value and control threshold.Conclusion This method has high sensitivity and good accuracy,which can be used for the content determination of 36 inorganic element impurities in Montmorillonite Powder.

关 键 词：蒙脱石散 电感耦合等离子体质谱法 微波消解法 无机元素杂质 质量控制 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学] R286.0