LC-MS/MS法测定红景天胶囊中红景天苷含量的方法
投稿时间:2020-07-23  修订日期:2021-03-13  点此下载全文
引用本文:方慧君,段烨,张春丽,黄隆基,王荣.LC-MS/MS法测定红景天胶囊中红景天苷含量的方法[J].药学实践杂志,2021,39(2):157~159
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作者单位E-mail
方慧君 中国人民解放军联勤保障部队第九四〇医院药剂科甘肃 兰州 730050  
段烨 中国人民解放军联勤保障部队第九四〇医院药剂科甘肃 兰州 730050  
张春丽 中国人民解放军联勤保障部队第九四〇医院药剂科甘肃 兰州 730050  
黄隆基 中国人民解放军联勤保障部队第九四〇医院药剂科甘肃 兰州 730050  
王荣 中国人民解放军联勤保障部队第九四〇医院药剂科甘肃 兰州 730050 wangrong-69@163.com 
基金项目:国家自然科学基金(81673508),军队后勤科研面上项目(CLB19J049)
中文摘要:目的 建立LC-MS/MS测定红景天胶囊中红景天苷的方法。方法 通过电喷雾离子源(ESI),采用多反应检测方式进行负离子检测,以茶碱为内标,用于定量分析的红景天苷、茶碱的检测离子分别为m/z 299.0→119.0和m/z 178.8→164.0。采用Shim-pack XR-ODS 柱(3.0 mm×75 mm,2.0 μm)分离,以乙腈∶5 mmol/L乙酸铵溶液(90∶10,V/V)为流动相,流速为0.40 ml/min,柱温为25 ℃。结果 在3 min内完成红景天苷含量分析,线性范围为10~2 000 ng/ml,最低检测限为10 ng/ml。结论 该方法重复性好、灵敏度高、分析速度快、操作简单,可作为红景天胶囊中红景天苷含量的测定方法,适用于药物质量检验,方便安全用药。
中文关键词:红景天苷  红景天胶囊  液相色谱串联质谱法
 
LC-MS/MS method for determination of salidroside in the capsule
Abstract:Objective To establish a LC-MS/MS method for the determination of salidroside in the capsule.Methods An electrospray ionization and multiple reaction detection were used to detect negative ion. Theophylline was used as standard. The detection ions of salidroside and theophylline used for quantitative analysis were m/z 299.0→119.0, and m/z 178.8→164.0, respectively. The Shim-pack XR-ODS (3.0 mm×75 mm, 2.0 μm) column was used for separation. The mobile phase was acetonitrile: 5 mmol/L ammonium acetate solution (90∶10, V/V). The flow rate was 0.40 ml/min. The column temperature was 25 ℃.Results The content of salidroside was analyzed within 3 minutes. The linear range was 10–2 000 ng/ml, and the minimum detection limit was 10 ng/ml.Conclusion The method has good repeatability, high sensitivity, fast analysis speed and simple operation. It can be used as a method for the determination of salidroside in the capsule. It is suitable for the quality inspection of drugs and convenient for safe use.
keywords:salidroside  salidroside capsule  LC-MS/MS
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