电感耦合等离子体-质谱法测定艾司唑仑片中7种元素杂质含量  

Content Determination of Seven Elemental Impurities in Estazolam Tablets by ICP-MS

作　　者：胡幸 匡鑫玉 曾令高 HU Xing;KUANG Xinyu;ZENG Linggao(Chongqing Institute for Food and Drug Control·NMPA Key Laboratory for 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》2024年第9期7-10,共4页China Pharmaceuticals

基　　金：重庆市技术创新与应用发展专项面上项目[CSTB2022TIAD-GPX0071]。

摘　　要：目的建立测定艾司唑仑片中1类元素砷(As)、镉(Cd)、汞(Hg)、铅(Pb)及2A类元素钴(Co)、镍(Ni)、钒(V)杂质含量的电感耦合等离子体-质谱(ICP-MS)法。方法采用硝酸前处理样品。等离子体射频功率为1500 W,雾化气流速为0.92 L/min,蠕动泵速为25 r/min,碰撞模式为动能歧视(KED)模式,碰撞气为氦气,碰撞气流速为3.8 mL/min,以铟(^(115)In)和铋(^(209)Bi)元素为内标元素校正基体效应和干扰。结果As,Cd,Hg,Pb,Co,Ni,V元素的质量浓度分别在0~4.5 ng/mL、0~1.5 ng/mL、0~9.0 ng/mL、0~1.5 ng/mL、0~15.0 ng/mL、0~60.0 ng/mL、0~30.0 ng/mL范围内与待测元素和内标元素响应值的比值线性关系良好(r≥0.9994,n=5);重复性、中间精密度试验结果的RSD均小于4%(n=6);加样回收率分别为96.33%,90.02%,89.46%,105.08%,104.43%,99.07%,106.04%,RSD分别为4.48%,4.42%,3.19%,4.58%,2.16%,2.43%,1.87%(n=9)。20批样品中7种元素杂质的含量均远低于限度。结论该方法操作简单、结果准确,可用于艾司唑仑片中1类和2A类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 category 1 elements[arsenic(As),cadmium(Cd),hydrargyrum(Hg),and lead(Pb)],and category 2A elements[cobalt(Co),nickel(Ni),and vanadium(V)]in Estazolam Tablets.Methods The samples were pre-treated with the nitric acid.The radio frequency(RF)power of the plasma was 1500 W,the flow rate of the atomized gas was 0.92 L/min,the speed of the peristaltic pump was 25 r/min,the crash mode was kinetic energy discrimination(KED)mode,the collision gas was helium with a flow rate of 3.8 mL/min.The matrix effect and interference were corrected with indium(^(115)In)and bismuth(^(209)Bi)elements as internal standards.Results The linear ranges of As,Cd,Hg,Pb,Co,Ni,and V elements were 0-4.5 ng/mL,0-1.5 ng/mL,0-9.0 ng/mL,0-1.5 ng/mL,0-15.0 ng/mL,0-60.0 ng/mL,and 0-30.0 ng/mL(r≥0.9994,n=5),respectively.The RSDs of the repeatability and intermediate precision test results were lower than 4%(n=6).The recovery rates of the above seven elemental impurities were 96.33%,90.02%,89.46%,105.08%,104.43%,99.07%,and 106.04%,with RSDs of 4.48%,4.42%,3.19%,4.58%,2.16%,2.43%,and 1.87%(n=9),respectively.The impurity content of seven elemental impurities in 20 batches of samples was far below the specified limits.Conclusion The method is simple and accurate,which can be used for the content determination of category 1 and 2A elemental impurities in Estazolam Tablets.

关 键 词：电感耦合等离子体质谱法 艾司唑仑片 元素杂质 含量测定 

分 类 号：R927.2[医药卫生—药学] R971