ICP-MS法测定左氧氟沙星注射液中10种元素杂质的含量  

Determination of 10 elemental impurities in levofloxacin injection by ICP-MS

作　　者：钟思伟 ZHONG Si-wei(Anhui Biochem Pharmaceutical Co.,Ltd.,Hefei 230031,China)

机构地区：[1]安徽贝克生物制药有限公司,合肥230031

出　　处：《药物分析杂志》2023年第11期1914-1919,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立电感耦合等离子体质谱法测定左氧氟沙星注射液中锂(Li)、钒(V)、钴(Co)、镍(Ni)、铜(Cu)、砷(As)、镉(Cd)、锑(Sb)、汞(Hg)、铅(Pb)10种元素杂质的含量。方法:选择氦气碰撞结合动能甄别模式(KED);RF功率1 550 W;采样深度5 mm;载气(氩气)流量1.13 L·min^(-1);辅助气流量0.8 L·min^(-1);积分时间0.03 s,采集次数30次;以铟(In)、锗(Ge)、钪(Sc)、铋(Bi)作为内标,按照标准曲线法同时测定上述10种元素杂质的含量。结果:上述10种元素杂质的响应值和其质量浓度均呈良好的线性关系(r>0.99);加样回收率均在90%~110%范围内;重复性RSD<6%;检测限和定量限均远小于各元素杂质的限度;检测条件(载气流量)在一定范围内(1.05~1.20 L·min^(-1))的变化对测定结果无显著影响;供试品溶液室温放置3 d内各元素测得值的RSD<6%,溶液稳定性良好;3家不同企业生产的左氧氟沙星注射液中10种元素杂质的测定结果均符合规定。结论:经分析方法学验证,该方法准确专属,快速灵敏,适用于左氧氟沙星注射液中10种元素杂质的检查。Objective:To establish a method for the determination of lithium(Li),vanadium(V),cobalt(Co),nickel(Ni),copper(Cu),arsenic(As),cadmium(Cd),antimony(Sb),mercury(Hg)and lead(Pb)in levofloxacin injection by inductively coupled plasma mass spectrometry(ICP-MS).Methods:Helium collision combined with kinetic energy discrimination(KED)mode was selected.The RF power was 1550 W and the sampling depth was 5 mm,the carrier gas(Argon)flow was 1.13 L·min^(-1)and the auxiliary gas flow was 0.8 L·min^(-1).The integration time was 0.03 s and the acquisition times were 30 times.Indium(In),germanium(Ge),scandium(Sc)and bismuth(Bi)were used as internal standards.Contents of the above 10 elemental impurities were simultaneously determined according to the calibration curves by ICP-MS.Results:The response values of the above 10 elemental impurities and their mass concentrations were in good linear relationships(every correlation coefficient r was greater than 0.99).The recovery rates were in the ranges of 90%to 110%.The RSDs of repeatability were less than 6%,the limit of detection and the limit of quantification were smaller than the limit of each elemental impurity.The change of detection conditions(flow rate)in a range of 1.05 L·min^(-1)to 1.20 L·min^(-1)had no significant effect on the results of measurement.The RSD of each element in the test solution which was stored at room temperature for 3 days was less than 6%.The stability of the test solution was good.The determination results of 10 elemental impurities in Levofloxacin Injection produced by three different companies were all in conformity with the regulations.Conclusion:Analytical method validation showed that the method is accurate,exclusive,rapid,sensitive and suitable for the determination of 10 elemental impurities in Levofloxacin Injection.

关 键 词：ICP-MS 左氧氟沙星注射液 元素杂质 记忆效应 分析方法验证 

分 类 号：R917[医药卫生—药物分析学]