摘要
目的:建立HPLC-ESI-MS/MS法同时测定血必净注射液中11种指标性成分的含量。方法:采用Agilent Extend-C_(18)柱(2.1 mm×100 mm,1.8μm),流动相为0.1%甲酸水-乙腈,梯度洗脱,流速为0.3 mL·min^(-1);质谱采用ESI正、负离子同时采集,多反应监测(MRM)模式扫描,测定含量。结果:在优化的色谱质谱条件下,11种成分分别在5.000~500.0、1.000~800.0、40.00~8000、4.000~800.0、10.00~8000、0.6250~500.0、0.5000~100.0、1.000~800.0、10.00~500.0、2.000~800.0、1.000~800.0 ng·mL^(-1)线性关系良好(r^(2)≥0.9961),平均加样回收率97.01%~102.70%(RSD≤6.4%);测定结果表明,11种成分在6个批次血必净注射液中含量较为稳定。结论:该方法简便、灵敏、高效,可用于血必净注射液中多种成分的快速测定,为其质量控制研究提供科学的依据。
Objective:To establish an HPLC-ESI-MS/MS method for simultaneous determination of 11 active or potential sensitizing components in Xuebijing injections.Methods:The chromatographic separation was achieved on an Agilent Extend-C_(18)(2.1 mm×100 mm,1.8μm)column;The mobile phase was consisted of 0.1%formic acid water-acetonitrile at a flow rate of 0.3 mL·min^(-1) with gradient elution,the mass spectrums were scanned by ESI+and ESI-multiple reaction monitoring(MRM)mode.Results:Under the optimized conditions,the 11 components showed good linear relationships in the ranges of 5.000-500.0,1.000-800.0,40.00-8000,4.000-800.0,10.00-8000,0.6250-500.0,0.5000-100.0,1.000-800.0,10.00-500.0,2.000-800.0 or 1.000~800.0 ng·mL^(-1),respectively(r^(2)≥0.9961),whose average recoveries were 97.01%-102.70%(RSD≤6.4%).The analysis results showed that the quantities of the 11 components were stable in six batches of Xuebijing injections.Conclusion:This simple,sensitive,and efficient method can be used for the rapid determination of multiple index components,which provide a scientific basis for the quality control research of Xuebijing injections.
作者
王红
刘玲
苏联麟
郭志花
崔永伟
WANG Hong;LIU Ling;SU Lianlin;GUO Zhihua;CUI Yongwei(Department of Pharmacy,Nanjing Lishui District Hospital of TCM,Nanjing,Jiangsu 211200,China;Pharmacy College of Nanjing University of Chinese Medicine,Nanjing,Jiangsu 210046,China)
出处
《药学与临床研究》
2021年第4期246-250,共5页
Pharmaceutical and Clinical Research
基金
南京药学会-常州四药医院药学科研基金项目(2017YX013)
南京市中医药青年人才培养计划项目(ZYQ20059)。
