三七姜高效液相色谱指纹图谱建立及3种成分含量测定  

Establishment of HPLC Fingerprints for Stahlianthus involucratus and Content Determination of Three Components

作　　者：梁洁 祁金丽 杨川川 胡珏 陈辉华 曹玉嫔 李耀华 孙正伊[4] LIANG Jie;QI Jinli;YANG Chuanchuan;HU Jue;CHEN Huihua;CAO Yupin;LI Yaohua;SUN Zhengyi(School of Pharmacy,Guangxi University of Chinese Medicine,Nanning 530200,China;Guangxi Zhuang Yao Medicine Center of Engineering and Technology,Nanning 530200, China;Guangxi Superior Chinese Patent Medicine and National Medicine Development Engineering Technology Center,Nanning 530200,China;Department of Pharmacy,Ruikang Hospital Affiliated to Guangxi University of Chinese Medicine,Nanning 530011,China)

机构地区：[1]广西中医药大学药学院,南宁530200 [2]广西壮瑶药工程技术研究中心,南宁530200 [3]广西优势中成药与民族药开发工程技术研究中心,南宁530200 [4]广西中医药大学附属瑞康医院药学部,南宁530011

出　　处：《医药导报》2022年第5期687-692,共6页Herald of Medicine

基　　金：广西自然科学基金资助项目(2020GXNSFAA238026);广西壮瑶药重点实验室项目(GXZYZZ2020-05);广西高等学校千名中青年骨干教师培育计划(桂教人〔2019〕5号);广西一流学科建设项目(桂教科研〔2018〕12号);广西壮瑶药协同创新中心项目(桂教科研〔2013〕20号);广西壮瑶药重点实验室培育基地项目(桂科基字〔2014〕32号);广西第八批自治区特聘专家项目(桂人才通字〔2019〕13号);广西高等学校高水平创新团队及卓越学者计划项目(桂教师范〔2019〕52号);广西科技基地和人才专项(桂科AD20238058);南宁市重点研发计划项目(20193115)。

摘　　要：目的采用高效液相色谱法(HPLC)建立壮药三七姜药材的指纹图谱,并测定其中原儿茶酸、对羟基苯甲酸和对羟基苯甲醛的含量。方法Phenomenex Kinetex XB-C_(18)色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈-0.1%磷酸,梯度洗脱,检测波长为220 nm,流速0.8 mL·min^(-1),柱温35℃,进样量15μL。以莪术二酮作为参照峰,建立10批三七姜药材的指纹图谱,综合应用相似度评价,聚类分析(HCA)和主成分分析(PCA)评价三七姜药材批间质量差异。同法测定10批三七姜药材原儿茶酸、对羟基苯甲酸和对羟基苯甲醛的含量。结果10批样品中有16个共有峰,相似度均>0.9。聚类分析可将样品分为3类,筛选出3个主成分因子,累计贡献率93.875%。原儿茶酸、对羟基苯甲酸和对羟基苯甲醛在测定范围内(2.36~16.52,2.12~14.84,1.49~10.43μg·mL^(-1))呈良好的线性关系;平均加样回收率分别为101.50%,101.54%,100.67%,RSD分别为1.85%,1.81%,1.54%;10批三七姜药材中原儿茶酸、对羟基苯甲酸和对羟基苯甲醛的含量分别为0.3321~1.4642,0.4757~1.3450,0.3306~1.0465 mg·g^(-1)。结论该方法稳定可靠,可用于三七姜药材的质量控制。Objective To establish the high performance liquid chromatography(HPLC)fingerprint of Zhuang medicine Stahlianthus involucratus(King ex Bak.)Craib,and to determine the contents of protocatechuic acid,p-hydroxybenzoic acid and p-hydroxybenzaldehyde.Methods The Phenomenex Kinetex XB-C_(18) column(4.6 mm×250 mm,5μm)was used,and the mobile phase was acetonitrile-0.1%phosphoric acid in a gradient elution.The detection wavelength was 220 nm,the flow rate was 0.8 mL·min^(-1),the column temperature was 35℃,and the injection volume was 15μL.Using curdione as reference,HPLC fingerprints of 10 batches of Stahlianthus involucratus were established.Similarity analysis,hierarchical cluster analysis(HCA)and principal component analysis(PCA)were used to evaluate the quality difference between batches of Stahlianthus involucratus.The contents of protocatechuic acid,p-hydroxybenzoic acid and p-hydroxybenzaldehydein in 10 batches of Stahlianthus involucratus samples were determined by the same method.Results There were 16 common peaks in the 10 batches of Stahlianthus involucratus samples,and the similarity was more than 0.9.The samples were classified into three types according to CA.Three principal component factors were selected,and the cumulative contribution rate was 93.875%.Protocatechuic acid,p-hydroxybenzoic acid and p-hydroxybenzaldehyde showed a good linearity within the determined ranges(2.36-16.52,2.12-14.84,and 1.49-10.43μg·mL^(-1)),and the average recovery was 101.50%,101.54%,and 100.67%;RSD was 1.85%,1.81%,and 1.54%,respectively.The contents of protocatechuic acid,p-hydroxybenzoic acid and p-hydroxybenzaldehyde in 10 batches of Stahlianthus involucratus ranged from 0.3321-1.4642,0.4757-1.3450 and 0.3306-1.0465 mg·g^(-1),respectively.Conclusion The method is stable and reliable,which can be used for quality control of Stahlianthus involucratus.

关 键 词：三七姜 原儿茶酸 对羟基苯甲酸 对羟基苯甲醛 含量测定 指纹图谱 色谱法 高效液相 

分 类 号：R282.71[医药卫生—中药学] R927.2[医药卫生—中医学]