八珍益智方UPLC指纹图谱研究及多成分定量测定  

Study on UPLC fingerprint of Bazhen Yizhi prescription and quantitative determination of multiple components

作　　者：卜凡淑 牛阳[2] 黄楷迪 张婷[1] 张祎盈 任慧 钱大玮[3] 郭盛[3] 段金廒[3] BU Fan-shu;NIU Yang;HUANG Kai-di;ZHANG Ting;ZHANG Yi-ying;REN Hui;QIAN Da-wei;GUO Sheng;DUAN Jin-ao(Jiangsu Collaborative Innovation Center of Chinese Medicinal Resources Industrialization/Jiangsu Key Laboratory for High Technology Research of Traditional Chinese Medicine Formulae,Nanjing University of Chinese Medicine,Nanjing 210023,China;Key Laboratory of Hui Ethnic Medicine Modernization,Ministry of Education,Ningxia Medical University,Yinchuan 750001,China;National University of Traditional Chinese Medicine National Industrial Engineering Research Center for the Industrialization of Traditional Chinese Medicine Resources and Fonnula Innovation Drugs,Nanjing 210023,China)

机构地区：[1]南京中医药大学江苏省中药资源产业化过程协同创新中心/江苏省方剂高技术研究重点实验室,南京210023 [2]宁夏医科大学,回医药现代化教育部重点实验室,银川750001 [3]南京中医药大学中药资源产业化与方剂创新药物国家地方联合工程研究中心,南京210023

出　　处：《药物分析杂志》2021年第10期1707-1717,共11页Chinese Journal of Pharmaceutical Analysis

基　　金：宁夏回族自治区重点研发计划(东西部科技合作)项目(2017BY084)。

摘　　要：目的:采用超高效液相色谱(UPLC)建立八珍益智方指纹图谱和多成分定量分析方法。方法:采用ACQUITY UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8μm),流动相为乙腈(A)-0.2%甲酸水溶液(B),梯度洗脱,流速0.4 mL·min^(-1),检测波长254 nm(甘草酸)及300 nm(原儿茶酸、甘草苷、橙皮苷、异甘草苷、川陈皮素、桔皮素)。通过对照品比对与Q-TOF/MS技术对共有峰进行指认,采用UPLC-PAD进行含量测定。结果:测得10批次八珍益智方样品的指纹图谱与对照指纹图谱的相似度均大于0.936;共确定八珍益智方指纹图谱19个共有峰,指认14个化学成分,对其中原儿茶酸、甘草苷、橙皮苷、异甘草苷、川陈皮素、桔皮素、甘草酸7个成分进行含量测定。上述7个成分在一定浓度范围内呈良好线性关系,相关系数均大于0.9999;方法学考察结果显示各项指标均符合要求,回收率范围为92.8%~106.7%,RSD小于4.2%。10批样品中原儿茶酸、甘草苷、橙皮苷、异甘草苷、川陈皮素、桔皮素、甘草酸含量范围分别为0.006~0.017、0.035~0.220、0.622~2.113、0.015~0.045、0.007~0.022、0.003~0.010、0.237~0.642 mg·g^(-1)。结论:所建立的指纹图谱及多指标成分含量测定的分析方法稳定可行,专属性强,可用于八珍益智方的质量控制,为新药研发和临床安全用药提供依据。Objective:To establish the fingerprint and multi-component determination method of Bazhen Yizhi prescription by using ultra-high performance liquid chromatography(UPLC).Methods:ACQUITY UPLC HSS T3(100 mm×2.1 mm,1.8μm)column was used,the mobile phase was acetonitrile(A)-0.2%formic acid aqueous solution(B)with gradient elution at a flow rate of 0.4 mL·min^(-1),the detection wavelengths were 254 nm(glycyrrhizic acid)and 300 nm(3,4-dihydroxybenzoic acid,liquiritin,hesperidin,isoliquiritin,nobiletin,tangeretin).The common peaks were identified by comparison with reference substances and by Q-TOF/MS technology,and UPLC-PAD was used for content determination.Results:The similarity of fingerprints of 10 batches of Bazhen Yizhi prescription samples to reference fingerprint were all above 0.936.A total of 19 common peaks in the fingerprint of Bazhen Yizhi prescription were assigned,and 14 components were identified.The contents of 3,4-dihydroxybenzoic acid,liquiritin,hesperidin,isoliquiritin,nobiletin,tangeretin and glycyrrhizic acid were determined.The 7 substances showed good linear relationship within certain concentration ranges.The correlation coefficients were all above 0.9999.The methodological investigation results showed that all indicators meet the requirements,the recovery rates were between 92.8%-106.7%,and the RSDs were less than 4.23%.The content ranges of 3,4-dihydroxybenzoic acid,liquiritin,hesperidin,isoliquiritin,nobiletin,tangeretin and glycyrrhizic acid in 10 batches of samples were 0.006-0.017,0.035-0.220,0.622-2.113,0.015-0.045,0.007-0.022,0.003-0.010 and 0.237-0.642 mg·g^(-1),respectively.Conclusion:The fingerprint and the determination method of multi-index components are stable,feasible and specific,and can be used for the quality control of Bazhen Yizhi prescription,providing a basis for new drug development and clinical safe drug use.

关 键 词：八珍益智方 原儿茶酸 甘草苷 橙皮苷 异甘草苷 川陈皮素 桔皮素 甘草酸 指纹图谱 多组分定量测定 

分 类 号：R917[医药卫生—药物分析学]