HPLC-DAD-Q-TOF-MS/MS法的银黄颗粒主要成分定性与定量研究  

Qualitative and quantitative analysis of major constituents in Yinhuang Granules by HPLC-DAD-Q-TOF-MS / MS

作　　者：向青[1,2] 王小花[2] 林慧[2] 林婧[3] 许文[1,2,3] 

机构地区：[1]福建中医药大学生物医药研发中心,福建福州350122 [2]福建中医药大学药学院,福建福州350122 [3]福建中医药大学中西医结合研究院,福建福州350122

出　　处：《中成药》2015年第1期105-112,共8页Chinese Traditional Patent Medicine

基　　金：福建省卫生厅青年科研课题(2013-2-55);福建省"大学生创新创业训练计划"项目(3120403044)

摘　　要：目的采用高效液相色谱串联四极杆飞行时间质谱（HPLC-Q-TOF-MS/MS）快速鉴定银黄颗粒化学成分和HPLC-DAD法同时定量测定银黄颗粒中15种成分（獐牙菜苷、马钱苷、新绿原酸、绿原酸、隐绿原酸、咖啡酸、芦丁、异绿原酸B、异绿原酸A、异绿原酸C、野黄芩苷、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素）。方法分析采用月旭Ultimate-XB C18色谱柱（4.6 mm×150 mm,5μm）,流动相为乙腈-0.1%甲酸水,梯度洗脱,体积流量0.8 m L/min,柱温30℃。飞行时间质谱,采用负离子模式扫描。二极管阵列检测器的检测波长为240、276、326 nm。结果 HPLC-Q-TOF-MS/MS法推断鉴定银黄颗粒中的44种成分,HPLC-DAD定量分析银黄颗粒中15种成分在考察的质量浓度范围内,与峰面积之间呈良好的线性关系（r〉0.999 0）;回收率均在97.3%~100.9%范围内,RSD为1.4%~2.8%。结论通过HPLC-Q-TOF-MS/MS法和HPLC-DAD法鉴定银黄颗粒的化学成分优于HPLC法,尤其测定环烯醚萜苷类成分（獐牙菜苷、马钱苷）可为综合评价银黄制剂的质量提供参考。AIM To use a qualitative analytical method of liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry（ HPLC-Q-TOF-MS / MS） for identification of multi-constituent and HPLCDAD for simultaneously determining 15 major constituents（ neochlorogenic acid,chlorogenic acid,cryptochlorogenin acid,caffeic acid,sweroside,loganin,rutin,scutellarin,isochlorogenic acid B,isochlorogenic acid A,isochlorogenic acid C,baicalin,wogonoside,baicalein,wogonin） in Yinhuang Granules. METHODS The assay was performed on a Welch Ultimate XB-C18column（ 4. 6 mm × 150 mm,5 μm） with the mobile phase consisting of acetonitrile（ A） and water containing 0. 1% formic acid（ B） in gradient mode at a flow rate of 0. 8 m L / min. The column temperature was at 30 ℃ and the optimum detection wavelength of DAD was set at 240,276,and 326 nm.Q-TOF-MS used negative ion mode. RESULTS Forty-four constituents were identified in Yinhuang Granules by HPLC-Q-TOF-MS / MS. The fifteen constituents were quantitatively measured by HPLC-DAD and their linear ranges were fine（ r 〉 0. 999 0） with overall recoveries ranging from 97. 25% to 100. 86%,and the RSD ranging from1. 4% to 2. 8%. CONCLUSION HPLC-Q-TOF-MS / MS combined with HPLC-DAD for analysis are superior to HPLC,especially the measurement of iridoids（ sweroside,loganin）,and the method could be applied to the evaluation of Yinhuang preparations.

关 键 词：银黄颗粒 高效液相色谱串联四级杆飞行时间质谱 HPLC-DAD 化学成分 

分 类 号：R927.2[医药卫生—药学]