超高效液相色谱-质谱法同时测定双黄连胶囊中的3种有效成分  

Simultaneous determination of three effective components in shuanghuanglian capsules by ultra-high performance liquid chromatography-mass spectrometry

作　　者：张红伟 盛静[2] 陈伟光[2] 欧贝丽 屠捷红[2] 

机构地区：[1]浙江嘉兴市食品药品检验所,嘉兴314001 [2]浙江嘉兴学院医学院,嘉兴314001

出　　处：《海峡药学》2012年第6期36-39,共4页Strait Pharmaceutical Journal

基　　金：嘉兴市科技计划项目基金资助;基金编号:2009AY2064

摘　　要：目的建立了同时测定双黄连胶囊中的绿原酸、黄芩苷和连翘苷3种有效成分的超高效液相色谱-电喷雾电离质谱（HPLC-ESI/MS）分析方法。方法采用Waters BEH-C18色谱柱,以含0.2%甲酸的0.4mmol·L-1醋酸钠（A相）、甲醇（B相）为流动相进行梯度洗脱,在ESI正离子模式下,采用选择离子反应监测方法进行测定,用峰面积进行定量。结果绿原酸、黄芩苷和连翘苷的线性范围分别0.05~50mg.L-1,0.10~500mg.L-1和0.01~25mg.L-1;检出限分别为0.010,0.020,0.002mg.L-1。3种成分的加样回收率为97.2%~101.6%,相对标准偏差小于2.3%。结论该法快捷、准确、重复性好,可用于双黄连胶囊中的3种有效成分含量的同时测定。OBJECTIVE To develope ultra-high performance liquid chromatography-mass spectrometry（HPLC-ESI/MS） method for the Simultaneous determination of three effective components in shuanghuanglian capsule.METHODS The HPLC separation was performed on a Waters BEH-C18 column（1.7μm,2.1mm×100mm） using 0.4mmol·L-1 sodium acetate solution containing 0.2% formic acid（A） and acetonitrile（B） as the mobile phase with gradientelution（A%：20→25,0→3min;25→30,3→4min;30→35,4→26 min;35→80,26→28 min）at a flow rate of 0.2mL·min-1.The analytes were detected by ESI（＋）-M under selected ion reation mode（0~5min,m/z 377;19~21min,m/z 470;21~23min,m/z 558）,qualitificated by peak area.RESULTS The linear ranges were 0.05~50mg·L-1,0.10~500mg·L-1 and 0.01~25mg·L-1,with detection limits of 0.010,0.020,0.002mg·L-1 for chlorogenic acid,baicalin,forsythin respectively.The average recoveries ranged from 97.2%~101.6%,The relative standard deviation were less than 2.3%.CONCLUSION This method is rapid,accurate,and suitable for the quality control of the three effective components in shuanghuanglian capsule.

关 键 词：超高效液相色谱-质谱法 绿原酸 黄芩苷 连翘苷 双黄连胶囊 

分 类 号：R927.2[医药卫生—药学]