HPLC-ELSD结合化学计量学研究银杏叶片中萜类内酯指纹图谱  

Fingerprint Analysis of Terpene Lactones in Ginkgo Biloba Tablets by HPLC-ELSD Coupled with Chemometrics

作　　者：吴雨龙[1,2,3] 李艳静[1,3] 王佩香[1,3] 丁岗[1,3] 李萍[2] 段金廒[4,3] 萧伟[1,3] 

机构地区：[1]江苏康缘药业股份有限公司,连云港222001 [2]中国药科大学天然药物活性组分与药效国家重点实验室,南京210009 [3]中药制药过程新技术国家重点实验室,连云港222001 [4]南京中医药大学/江苏省方剂研究重点实验室,南京210046

出　　处：《世界科学技术-中医药现代化》2013年第9期1952-1958,共7页Modernization of Traditional Chinese Medicine and Materia Medica-World Science and Technology

基　　金：江苏省科技厅科技成果转化项目(BA2010109):缺血性中风治疗药物银杏内酯注射液的研发及产业化;负责人:萧伟;科学技术部国家科技支撑计划(2011BAI04B03):华东区中药材规范化种植及大宗中药材综合开发技术研究--银杏叶系列产品质量标准提升及银杏资源综合开发利用;总课题负责人:段金廒;子课题负责人:萧伟

摘　　要：目的:建立不同厂家银杏叶片中萜类内酯成分HPLC-ELSD指纹图谱。方法:色谱柱为Agilent Extend-C18(4.6 mm×250 mm,5μm),流动相为正丙醇-四氢呋喃-水(1∶15∶84),柱温为30℃,流速为1mL·min-1,蒸发光散射检测器检测;采用LC/Q-TOF MS对指纹图谱中的共有峰进行指认。并利用化学计量学方法,包括主成分分析(PCA)、相似度分析(SA)、聚类分析(HCA),对色谱数据进行分析。结果:该方法精密度、稳定性、重复性良好。同时采用LC/Q-TOF MS方法指认了5个共有峰,分别为银杏内酯J(M)、银杏内酯C、银杏内酯A、银杏内酯B及白果内酯。并采用该方法测定了市售14批银杏叶片,结合PCA、SA及HCA生成了银杏叶片中萜类内酯对照指纹图谱,并根据质量差异将样品分为4大类。结论:本方法可用于银杏叶片中萜类内酯成分的质量评价。This study was aimed to establish a high performance liquid chromatography （HPLC） method coupled with Evaporative Light-scattering Detector （ELSD） in order to develop the determination of fingerprint of terpene lactones in Ginkgo biloba tablets. An Agilent Extend-C18 （4.6 mm× 250 mm, 5μm） was employed as the analysis column and the normal propyl alcohol-tetrahydrofuran-water （1：15：84） as mobile phase. The column temperature was 30℃. And the flow rate was 1.0 mL·min-1. HPLC coupled with eleetrospray ionization quadrupole time-of-flight tandem mass spectrometry （Q-TOF MS） was used to identify the common peaks. The fingerprint was further evaluated by chemometrics methods including principal component analysis （PCA）, similarity analysis （SA） and hierarchical clus- tering analysis （HCA）. The results showed that the precision, stability and repeatability of this method were favorable. Five common peaks were identified by LC/Q-TOF MS as ginkgolide J （M）, C, A, B and bilobalide, respectively Fourteen batches of Ginkgo biloba tablets were determined. With the aid of PCA, SA and HCA, the common pattem of the fingerprint of terpene lactones was established. Samples were divided into 4 clusters by their quality differ- ence. It was concluded that the method established in this paper can be used for quality evaluation of terpene lac- tones in Ginkgo biloba tablets.

关 键 词：银杏叶片 萜类内酯HPLC-ELSD 指纹图谱化学计量学 质量评价 

分 类 号：R284[医药卫生—中药学]