HPLC-DAD-ESI-TOF/MS鉴别和测定前列欣胶囊中多种成分及其多指标定量指纹图谱研究  

Identification and determination of multiple components in Qianliexin capsules by HPLC-ESI-TOF/MS and study on the quantitative fingerprint

作　　者：赵志国[1] 张晓梦 张敏敏 刘敏 闫慧娇 王涛[1] 王晓[1] 耿岩玲[1] 赵恒强[1] 段文娟[1] ZHAO Zhi-guo ZHANG Xiao-meng ZHANG Min-min LIU Min YAN Hui-jiao WANG Tao WANG Xiao GENG Yan-ling ZHAO Heng-qiang DUAN Wen-juan(Shandong Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Process Control Research Center of Traditional Chinese Medicine of Shandong Academy of Sciences, Jinan 250014, China Shandong Hongjitang Pharmaceutical Limited Company, Jinan 250100, China)

机构地区：[1]山东省中药质量控制技术重点实验室山东省科学院中药过程控制研究中心山东省分析测试中心,济南250014 [2]山东宏济堂制药集团有限公司,济南250100

出　　处：《药物分析杂志》2017年第10期1810-1816,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：山东省科技发展计划(2016GSF202020);山东省自然科学基金(ZR2013HL029);山东省科学院科技发展基金项目(2012015);泰山学者岗位资助(郭兰萍);山东省科学院先导项目(郭兰萍)

摘　　要：目的:高效液相色谱-电喷雾飞行时间质谱(HPLC-ESI-TOF/MS)联用技术用于前列欣胶囊多种化学成分快速鉴定和测定及多指标定量指纹图谱研究。方法:采用Kromasil 100-5C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.8%甲酸流动相体系进行梯度洗脱,流速0.8 mL·min^(-1),柱温25℃,检测波长300 nm;利用ESI-TOF/MS法对前列欣胶囊提取物中多种化合物进行鉴别,对已知的活性成分进行定量测定,并建立前列欣胶囊的HPLC指纹图谱。结果:应用HPLC-DAD-ESI-TOF/MS指认了前列欣胶囊提取物中的8个成分(没食子酸、绿原酸、咖啡酸、王不留行黄酮苷、异槲皮苷、丹酚酸B、丹酚酸A、隐丹参酮),定量测定结果表明各化合物线性关系良好(r=0.999 0~0.999 7);平均回收率分别为95.25%、96.85%、98.10%、96.71%、97.87%、95.80%、97.57%和96.74%。10批样品中上述各化合物的质量分数分别为194.39~209.43、242.65~253.32、82.79~86.46、132.45~146.80、169.08~188.13、402.36~429.87、595.75~637.11、112.78~122.92μg·g^(-1);10批样品的相似度在0.999 6~1.000 0之间。结论:本研究所建立的活性成分快速鉴别和多指标定量指纹图谱测定方法,为提高前列欣胶囊的质量控制水平提供了技术支持。Objective：To establish a high performance liquid chromatography-electrospray time-of-flight mass spectrometry（HPLC-ESI-TOF/MS） method for rapid identification and determination of multiple components in Qianliexin capsules,and to establish the quantitative fingerprint. Methods：Separation was carried on Kromasil 100-5 C18 column using acetonitrile-0.8% formic acid as mobile phase at the flow rate of 1 mL·min-1 for gradient elution and the detection wavelength was 300 nm. The column temperature was set at 25 ℃. ESI-TOF/MS was used for identification of chemical ingredients in Qianliexin Capsules. Assay of multi-components in Qianliexin capsules and its fingerprint were established. Results：Eight ingredients（gallic acid,chlorogenic acid,caffeic acid,vaccarin,isoquercitrin,salvianolic acid B,salvianolic acid A and cryptotanshinone） were identified by the developed HPLC-DAD-ESI-TOF/MS method. Results of assay showed that good linearity（r=0.999 0-0.999 7） was found for the 8 compounds. And the average recoveries of gallic acid,chlorogenic acid,caffeic acid,vaccarin,isoquercitrin,salvianolic acid B,salvianolic acid A and cryptotanshinone were 95.25%,96.85%,98.10%,96.71%,97.87%,95.80%,97.57% and 96.74%,respectively. The contents of the above compounds in 10 samples were in the ranges of 194.39-209.43 μg·g-1,242.65-253.32 μg·g-1,82.79-86.46 μg·g-1,132.45-146.80 μg·g-1,169.08-188.13 μg·g-1,402.36-429.87 μg·g-1,595.75-637.11 μg·g-1 and 112.78-122.92 μg·g-1,respectively. And the similarity values of 10 batches of samples ranged from 0.999 6 to 1.000 0. Conclusion：The proposed method for rapid identification and multi-component quantitative fingerprint provided technology support for the quality evaluation of Qianliexin capsules.

关 键 词：前列欣胶囊 没食子酸 绿原酸 咖啡酸 王不留行黄酮苷 异槲皮苷 丹酚酸B 丹酚酸A 隐丹参酮 中药制剂多成分测定 指纹图谱 高效液相色谱-电喷雾飞行时间质谱 

分 类 号：R917[医药卫生—药物分析学]