摘要
目的:建立同时测定香连丸中小檗碱、药根碱、黄连碱、巴马汀、木香烃内酯、去氢木香内酯含量的高效液相色谱-质谱联用(HPLC-MS/MS)的检测方法。方法:采用Hypersil GOLD C 18色谱柱(50 mm×2.1 mm,3μm,Thermo),流动相为乙腈-0.1%甲酸水,梯度洗脱,流速为0.5 mL·min-1,进样量2μL,柱温25℃,采用ESI离子源在正离子模式下选择离子扫描模式进行定量分析。结果:小檗碱、药根碱、黄连碱、巴马汀、木香烃内酯、去氢木香内酯分别在83.871~934.163、39.939~480.298、42.371~461.046、42.982~473.626、42.193~510.321、41.785~512.478 ng·mL-1与峰面积呈现良好的线性关系,r均大于0.99,平均加样回收率分别为99.08%、98.80%、98.86%、99.11%、99.06%、99.40%,RSD分别为0.73%、0.78%、0.86%、0.76%、0.98%、1.03%。结论:所建立的方法简便、准确,可用于香连丸中主要成分的含量测定。
Objective:To develop a HPLC-MS/MS method for determination of berberine,jatrorrhizine,coptisine,palmatine,costunolide and dehydrocostus lactone in Xianglian Pills.Methods:The analysis was performed on a Hypersil GOLD C 18 column(50 mm×2.1 mm,3μm,Thermo)with gradient elution of acetonitrile-0.1%formic acid aqueous solution,and the flow rate was 0.5 mL·min-1.The injection volume was 2μL and the column temperature was 25℃.ESI ion source was used to select ion scanning mode for quantitative analysis in positive ion mode.Results:The linear ranges of berberine,jateorhizine,coptisine,palmatine,costunolide and dehydrocostus lactone were 83.871-934.163,39.939-480.298,42.371-461.046,42.982-473.626,42.193-510.321,41.785-512.478 ng·mL-1(r>0.99),respectively.The average recovery rates were 99.08%,98.80%,98.86%,99.11%,99.06%,99.40%,respectively,and the RSD were 0.73%,0.78%,0.86%,0.76%,0.98%,1.03%,respectively.Conclusion:This method is simple,accurate,and reliable to determine the contents of the main components in Xianglian Pills for the quality control.
作者
卢敏
熊山
牟艳玲
LU Min;XIONG Shan;MU Yan-ling(School of Medicine and Life Sciences,University of Jinan-Shandong Academy of Medical Sciences,Jinan 250200,China;Institute of Materia Medica,Shandong First Medical University&Shandong Academy of Medical Sciences,Jinan 250062,China;Key Laboratory for Biotech-Drugs Ministry of Health,Jinan 250062,China;Key Laboratory for Rare&Uncommon Diseases of Shandong Province,Jinan 250062,China)
出处
《中国现代中药》
CAS
2019年第12期1710-1714,共5页
Modern Chinese Medicine
基金
山东省自主创新及成果转化专项(2014ZZCX02105)
山东省医学科学院医药卫生科技创新工程
关键词
香连丸
液质联用
含量测定
生物碱
木香烃内酯
去氢木香内酯
Xianglian Pills
HPLC-MS/MS
content determination
alkaloid
costunolide
dehydrocostus lactone
