基于高效液相色谱指纹图谱和多成分定量的大蓟配方颗粒质量评价  

Quality Evaluation of Cirsium Japonicum Formula Granules Based on HPLC Fingerprints and Multi-Components Determination

作　　者：丁富娟 刘斌 赵海燕 张明 张力伟 王煦辰 张军鹏 孔令红 DING Fujuan;LIU Bin;ZHAO Haiyan;ZHANG Ming;ZHANG Liwei;WANG Xuchen;ZHANG Junpeng;KONG Linghong(Tai'an Testing Institute for Food and Drug Control,Tai'an,Shandong,China 271000;Daiyue District Center for Disease Control and Prevention,Tai'an,Shandong,China 271000)

机构地区：[1]山东省泰安市食品药品检验检测研究院,山东泰安271000 [2]山东省泰安市岱岳区疾病预防控制中心,山东泰安271000

出　　处：《中国药业》2024年第19期95-101,共7页China Pharmaceuticals

基　　金：山东省食品药品监督管理局2022年药品质量安全风险监测项目[2022-12]。

摘　　要：目的评价不同生产企业不同批次大蓟配方颗粒的质量。方法采用高效液相色谱(HPLC)法测定大蓟配方颗粒中5种有效成分的含量,色谱柱为Agilent Extend C18柱(250 mm×4.6 mm,5µm),流动相为乙腈-甲醇(4∶1,V/V)-0.1%磷酸溶液(梯度洗脱),流速为1.0 mL/min,检测波长为330 nm,柱温为30℃,进样量为10µL;建立指纹图谱,通过比对鉴定共有峰,并进行相似度评价,采用聚类分析法(CA)、主成分分析(PCA)法和正交偏最小二乘判别分析(OPLS-DA)法对5个生产企业的17批样品进行分析。结果大蓟配方颗粒的指纹图谱有14个共有峰,指认出了8个峰;CA和PCA将17批大蓟配方颗粒分为4类;OPLS-DA确定了6种差异标志物成分,对其影响显著性排序分别为芹菜素-7-O-葡萄糖醛酸苷>峰7>绿原酸>峰9>隐绿原酸>柳穿鱼叶苷。5种成分在各自质量浓度范围内与峰面积线性关系良好(r≥0.9991,n=5);平均加样回收率为95.88%~99.12%,RSD为1.40%~2.00%(n=9)。结论该方法操作简单,方法学考察结果良好,能用于大蓟配方颗粒的质量评价。Objective To evaluate the quality of different batches of Cirsium Japonicum Formula Granules(CJFG)from different manufacturers.Methods High-performance liquid chromatography(HPLC)method was used for the content determination of five active ingredients in CJFG,the chromatographic column was Agilent Extend C18 column(250 mm×4.6 mm,5µm),the mobile phase was acetonitrile methanol(4∶1,V/V)-0.1%phosphoric acid solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was 330 nm,the column temperature was 30℃,and the injection volume was 10µL.The fingerprints of CJFG were established to identify common peaks through comparison,and evaluate similarity.Cluster analysis(CA),principal component analysis(PCA),and orthogonal partial least squares-discriminant analysis(OPLS-DA)were used to analyze 17 batches of samples from five manufacturers.Results The fingerprints of CJFG had fourteen common peaks,and eight peaks were identified.CA and PCA results divided 17 batches of CJFG into four categories.OPLS-DA identified six differential marker components,and the order of their significance was apigenin-7-O-glucuronide>peak 7>chlorogenic acid>peak 9>cryptochlorogenic acid>pecaalinarin.The five components had a good linear relationship with peak area within their respective mass concentration ranges(r≥0.9991,n=5).The average recovery rate was in the range of 95.88%-99.12%,with RSD of 1.40%-2.00%(n=9).Conclusion The method is simple,and the results of methodological investigation are good,which can be used for the quality evaluation of CJFG.

关 键 词：大蓟配方颗粒 高效液相色谱指纹图谱 多成分定量 聚类分析法 主成分分析法 正交偏最小二乘判别分析法 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学] R286.0