电感耦合等离子体质谱法测定咪达唑仑注射液中18种元素杂质含量  

Content Determination of Eighteen Types of Elements in Midazolam Injection by ICP-MS

作　　者：胡幸 沈丹丹 匡鑫玉 陈丹丹 张伟 HU Xing;SHEN Dandan;KUANG Xinyu;CHEN Dandan;ZHANG Wei(Chongqing Institute for Food and Drug Control·NMPA Key Laboratory of Quality Monitoring of Narcotic Drugs and Psychotropic Substances,Chongqing,China 401121;College of Bioengineering,Chongqing University,Chongqing,China 400044)

机构地区：[1]重庆市食品药品检验检测研究院·国家药品监督管理局麻醉精神药品质量监测重点实验室,重庆401121 [2]重庆大学生物工程学院,重庆400044

出　　处：《中国药业》2023年第19期22-25,共4页China Pharmaceuticals

摘　　要：目的建立测定咪达唑仑注射液中镁(Mg)、铝(Al)、钛(Ti)、钒(V)、铬(Cr)、锰(Mn)、铁(Fe)、钴(Co)、镍(Ni)、铜(Cu)、锌(Zn)、砷(As)、锶(Sr)、镉(Cd)、锑(Sb)、钡(Ba)、汞(Hg)、铅(Pb)18种元素杂质含量的电感耦合等离子体质谱(ICP-MS)法。方法样品用含0.25%盐酸的3%硝酸溶液直接溶解,采用ICP-MS法测定。等离子体射频功率为1500 W,等离子体气、辅助气、雾化气、碰撞气流速分别为15,1.2,0.86,3.8 L/min,碰撞气为氦气,采集次数为3次。通过在线加入内标钪(^(45)Sc)、铟(^(115)In)、铼(^(187)Re)元素来监控和校正分析信号的短期和长期漂移。结果各元素在各自测定质量浓度范围内与待测元素和内标响应信号值的比值线性关系良好(r≥0.9990);精密度、稳定性、重复性试验结果的RSD均小于6%;加样回收率为86.80%~110.50%,RSD为1.56%~8.50%(n=9)。3批样品中均未检出Co,Cd,Sb,Hg,Pb,其余元素杂质含量均在规定范围内。结论该方法操作简单、结果准确,可用于咪达唑仑注射液中元素杂质的含量测定。Objective To establish an inductively coupled plasma-mass spectrometry(ICP-MS) method for the content determination of 18 elemental impurities in midazolam injection,including magnesium(Mg),aluminum(Al),titanium(Ti),vanadium(V),chromium(Cr),manganese(Mn),ferrum(Fe),cobalt(Co),nickel(Ni),cuprum(Cu),zinc(Zn),arsenic(As),strontium(Sr),cadmium(Cd),antimony(Sb),barium(Ba),hydrargyrum(Hg),and lead(Pb).Methods The samples were dissolved directly in3% HNO_(3)(0.25% HCl) and determined by ICP-MS.The radio frequency(RF) power of the plasma was 1 500 W,the flow rates of plasma gas,auxiliary gas,atomized gas and collision gas were 15,1.2,0.86 and 3.8 L/min,respectively,with collision gas of helium,and the repetition times were 3.By adding internal standard scandium(^(45)Sc),indium(^(115)In),and rhenium(^(187)Re)elements online,the short-term and long-term drift of the analysis signal was monitored and corrected.ResultsThe linear range of each element was good(r ≥ 0.999 0).The RSDs of precision,repeatability,and stability test results were all lower than 6%.The recovery rates of 18 elements were in the range of 86.80%-110.50% with RSDs of 1.56%-8.50%(n = 9).No Co,Cd,Sb,Hg,or Pb were detected in the three batches of samples,and the impurity content of other elements was within the specified limits.ConclusionThe method is simple and accurate,which can be used for the determination of elemental impurities in Midazolam Injection.

关 键 词：电感耦合等离子体质谱法 咪达唑仑注射液 元素杂质 含量测定 

分 类 号：R927.2[医药卫生—药学] R971