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 1 500 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(115In)和铋(209Bi)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≥0.999 4,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.
Abstract
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 1 500 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(115In)and bismuth(209Bi)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≥0.999 4,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.
基金项目
重庆市技术创新与应用发展专项面上项目(CSTB2022TIAD-GPX0071)
维普
万方数据