基于超高效液相色谱-紫外检测定量指纹图谱结合化学模式识别的复方金钱草颗粒质量评价  

Quality evaluation of Fufang Jinqiancao granules based on ultra performance liquid chromatography-ultraviolet detection quantitative fingerprint combined with chemical pattern recognition

作　　者：陆绍铭 徐鑫 薛倩倩 肖柳君 余文怡 魏彤 金红利 刘艳芳[1,2,3,4] 梁鑫淼 LU Shaoming;XU Xin;XUE Qianqian;XIAO Liujun;YU Wenyi;WEI Tong;JIN Hongli;LIU Yanfang;LIANG Xinmiao(Ganjiang Chinese Medicine Innovation Center,Nanchang 330000,China;Jiangxi Provincial Key Laboratory for Pharmacodynamic Material Basis of Traditional Chinese Medicine,Nanchang 330000,China;DICP-CMC Innovation Institute of Medicine,Taizhou 225300,China;Dalian Institute of Chemical Physics,Chinese Academy of Sciences,Dalian 116023,China)

机构地区：[1]赣江中药创新中心,江西南昌330000 [2]江西省中药药效物质基础重点实验室,江西南昌330000 [3]中科院大化所中国医药城生物医药创新研究院,江苏泰州225300 [4]中国科学院大连化学物理研究所,辽宁大连116023

出　　处：《色谱》2022年第12期1102-1110,共9页Chinese Journal of Chromatography

基　　金：中国科学院科技网络服务计划项目(KFJ-STS-QYZD-2021-03-004).

摘　　要：复方金钱草颗粒具有利尿、抑制泌尿系结石形成、抗炎、抗氧化作用,且具有较大的市场需求。因此,采用超高效液相色谱-紫外检测(UPLC-UV)法建立定量指纹图谱,并结合化学模式识别技术对不同年份的复方金钱草颗粒进行质量评价,可为其质量控制提供依据。采用聚类分析(HCA)和主成分分析(PCA)等化学模式识别技术对35批复方金钱草颗粒样品的指纹图谱数据进行分析,筛选出质量差异标志物芒果苷和异芒果苷,并对二者进行含量测定。在复方金钱草颗粒指纹图谱中共指认出12个共有峰,且35批样品的相似度均在0.952以上。在HCA中,将35批样品分为了两类,其中2018年和2019年的样品为一类,2020年和2021年的样品为一类。此外,PCA结果显示了与聚类分析相同的聚类趋势。在此基础上,进一步通过正交偏最小二乘法分析(OPLS-DA)筛选出了导致2018年、2019年与2020年、2021年的样品产生差异的差异标志物芒果苷和异芒果苷。以两个差异标志物芒果苷和异芒果苷为指标进行含量测定,结果显示色谱峰的分离度良好,线性关系良好,平均加标回收率分别为101.7%~105.6%和103.4%~105.5%,且相对标准偏差(RSD)均低于1.43%。在35批样品中,2020年、2021年的样品与2018年、2019年的样品相比,芒果苷与异芒果苷含量更高且波动范围更小。该研究建立了准确、可靠的复方金钱草颗粒质控方法,实现了对不同年份的复方金钱草颗粒样品合理、有效的质量评价,可为建立更系统、更全面的质量控制标准提供借鉴与参考。Fufang Jinqiancao granules have a large market demand due to the fact that they contain diuretics,inhibit urinary calculi formation,and exhibit both anti-inflammatory and antioxidant effects.In the current study,a fast and efficient quantitative ultra performance liquid chromatography-ultraviolet detection(UPLC-UV)fingerprinting method was established to analyze the Fufang Jinqiancao granules,while a chemical pattern recognition technology was used to evaluate the quality of the granules over different years.More specifically,the UPLC-UV system consisted of a Waters Acquity UPLC BEH C18 column(100 mm×2.1 mm,1.7μm),acetonitrile(mobile phase A),and a 0.1%formic acid aqueous solution(mobile phase B),wherein a gradient elution protocol was followed.Ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry(UPLC-Q-TOF-MS,Agilent InfinityⅡ1290-6545)was used in combination with reference substances and literature comparisons to identify the common peaks present in the quantitative fingerprint.The fingerprints of 35 batches of Fufang Jinqiancao granules were established by means of the quantitative UPLC-UV fingerprinting method,and the fingerprint data obtained for these samples were further analyzed by chemical pattern recognition techniques,including hierarchical cluster analysis(HCA)and principal component analysis(PCA).The quality difference markers,namely mangiferin and isomangiferin,were screened,and their contents were determined.It was found that 12 common peaks existed in the fingerprint of the Fufang Jinqiancao granules,and the similarities of all 35 batches of samples were greater than 0.952.In addition,for the purpose of HCA,the 35 batches were divided into two categories,of which sample years 2018 and 2019 belonged to one category,and sample years 2020 and 2021 belonged to another category.Notably,PCA gave the same clustering trends as HCA.Based on the obtained results,the mangiferin and isomangiferin components responsible for the differences between the 2018,2019 and 2020,2021

关 键 词：定量指纹图谱 相似度分析 聚类分析 主成分分析 正交偏最小二乘判别分析 芒果苷 异芒果苷 复方金钱草颗粒 

分 类 号：O658[理学—分析化学]