毛冬青饮片指纹图谱及定量分析
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摘要
目的:建立毛冬青饮片的HPLC-UV指纹图谱,同时测定46批次毛冬青饮片中毛冬青皂苷A_1和毛冬青皂苷B_1的含量,为毛冬青饮片的质量标准制定提供参考。方法:Kromasil C_(18)色谱柱(4. 6 mm×250 mm,5μm),流动相乙腈-0. 1%磷酸水溶液梯度洗脱,流速1. 0 mL·min~(-1),检测波长210 nm。采用中药色谱指纹图谱相似度评价系统(2012版)分析毛冬青指纹图谱,SPSS 20. 0软件对共有峰的峰面积进行聚类分析;主成分分析法对共有峰进行降维分析。结果:毛冬青饮片指纹图谱中根部位与枝部位差异较大,分别建立毛冬青根和枝的指纹图谱,并对共有峰进行聚类分析,聚类结果将根类毛冬青饮片聚为三类,枝类毛冬青饮片聚为二类;对比不同部位及不同产地间毛冬青饮片的整体性和差异性,主成分分析筛选出毛冬青饮片指纹图谱中起决定性作用的共有成分;建立毛冬青皂苷A_1,毛冬青皂苷B_1含量测定方法。结论:建立的毛冬青饮片指纹图谱和含量测定方法操作简便,适用性好,聚类分析和主成分分析筛选出毛冬青饮片质量控制的关键成分,研究结果可为毛冬青饮片质量控制提供参考。
Objective: To establish HPLC-UV fingerprints of Ilex pubescens pieces,and simultaneously determine two components in 46 batches of I. pubescens in pieces of I. pubescens saponin A_1 and B_1,in order to provide a reference for the quality standard of I. pubescens slices. Method: Methanol was used to extract the I. pubescens saponin samples,and the extracts were measured by HPLC-UV with the absorption wavelength at210 nm. Kromasil C_(18) column( 4. 6 mm × 250 mm,5 μm) was used for determining the extracts at a flow rate of1. 0 mL·min~(-1). The mobile phase condition was acetonitrile-0. 1% phosphoric acid aqueous solution with gradient mode. The chromatographic fingerprint similarity evaluation system of traditional Chinese medicine( 2012 edition)was used to analyze I. pubescens fingerprints. SPSS 20. 0 software was used to cluster the peak area of common peaks. Principal component analysis was performed to reduce the dimension of common peaks. Result: There were great differences between the root and stem parts in I. pubescens fingerprints. The fingerprints of roots and stems of I. pubescens were established respectively,cluster results assorted the roots of I. pubescens into three categories andthe branches of I. pubescens into two categories. The integrity and difference of I. pubescens decoction pieces from different parts and places of origin were compared,and the principal component analysis was performed to screen out the common components that played a decisive role in fingerprint of I. pubescens pieces. And the common peaks were determined. The content of saponin A_1 and saponin B_1 in Radix I. pubescens were determined.Conclusion: The established I. pubescens fingerprints and content determination methods are simple and suitable.Cluster analysis and principal component analysis are used to screen out the key components of quality control of I. pubescens. The results can provide references for quality control of I. pubescens.
Objective: To establish HPLC-UV fingerprints of Ilex pubescens pieces,and simultaneously determine two components in 46 batches of I. pubescens in pieces of I. pubescens saponin A_1 and B_1,in order to provide a reference for the quality standard of I. pubescens slices. Method: Methanol was used to extract the I. pubescens saponin samples,and the extracts were measured by HPLC-UV with the absorption wavelength at210 nm. Kromasil C_(18) column( 4. 6 mm × 250 mm,5 μm) was used for determining the extracts at a flow rate of1. 0 mL·min~(-1). The mobile phase condition was acetonitrile-0. 1% phosphoric acid aqueous solution with gradient mode. The chromatographic fingerprint similarity evaluation system of traditional Chinese medicine( 2012 edition)was used to analyze I. pubescens fingerprints. SPSS 20. 0 software was used to cluster the peak area of common peaks. Principal component analysis was performed to reduce the dimension of common peaks. Result: There were great differences between the root and stem parts in I. pubescens fingerprints. The fingerprints of roots and stems of I. pubescens were established respectively,cluster results assorted the roots of I. pubescens into three categories andthe branches of I. pubescens into two categories. The integrity and difference of I. pubescens decoction pieces from different parts and places of origin were compared,and the principal component analysis was performed to screen out the common components that played a decisive role in fingerprint of I. pubescens pieces. And the common peaks were determined. The content of saponin A_1 and saponin B_1 in Radix I. pubescens were determined.Conclusion: The established I. pubescens fingerprints and content determination methods are simple and suitable.Cluster analysis and principal component analysis are used to screen out the key components of quality control of I. pubescens. The results can provide references for quality control of I. pubescens.
引文
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[22]杨燚,师帅,魏丹,等.毛冬青中环烯醚萜苷类化学成分的分离与鉴定[J].沈阳药科大学学报,2017,34(8):634-639.
[2]吕一燕.毛冬青的临床应用研究[J].内蒙古中医药,2015,34(7):148-149.
[3]张帆,张小磊,苗明三.毛冬青总黄酮对大鼠血瘀合并脑缺血模型的影响[J].中国实验方剂学杂志,2012,18(22):187-191.
[4]张红蕊.浅谈毛冬青的临床应用[J].中国民康医学,2015,27(11):69-70.
[5]李向荣.毛冬青药理作用研究概述[J].环球中医药,2011,4(3):238-240.
[6]夏弘.毛冬青药理作用研究概述[J].工企医刊,2012,25(2):70.
[7]林培燕.毛冬青活性成分及其药代动力学研究[D].北京:北京协和医学院,2013.
[8]赵文珠,居文政,谈恒山.毛冬青中三萜皂苷类成分的研究进展[J].中医学报,2015,30(8):1181-1184.
[9]杨詹詹,付蓉.毛冬青的药理活性研究进展[J].山东化工,2017,46(24):77-78.
[10]湖南省食品药品监督管理局.湖南省中饮片标准[M].长沙:湖南科学技术出版社,2010:90.
[11]广东省食品药品监督管理局.广东省中饮片标准[M].广州:广东科技出版社,2011:77.
[12]江西省食品药品监督管理局.江西省中饮片标准[M].上海:上海科学技术出版社,2014:69.
[13]余成霞,柳文媛,冯锋,等.毛冬青药材的指纹图谱[J].药学学报,2009,44(4):1-6.
[14]朱明娟,邝国俊,高巍,等.毛冬青HPLC-UV指纹图谱与化学模式识别[J].中国中药杂志,2018,43(6):1182-1187.
[15]徐小娜.中药色谱指纹图谱研究及化学计量学方法的应用[D].长沙:中南大学,2010.
[16] SHI Y H,XIE Z Y,WANG R,et al. Quantitative and chemical fingerprint analysis for the quality evaluation of Isatis indigotica based on ultra-performance liquid chromatography with photodiode array detector combined with chemometric methods[J]. Int J Mol Sci,2012,13(12):9035-9050.
[17]孔浩,郭庆梅,王慧慧,等.主成分分析法在中药质量评价中的应用[J].辽宁中医杂志,2014,41(5):890-892.
[18]郝燕,董鸿晔,姜楠,等.基于主成分分析的中药色谱指纹图谱多维多息特征数据挖掘方法研究[J].中南药学,2007(3):267-272.
[19]应鸽,丁平,代蕾,等.毛冬青根和茎的HPLC指纹图谱研究[J].华西药学杂志,2013,28(5):506-509.
[20]周渊,李宁,张加余,等. RP-HPLC-DAD法同时测定毛冬青根中4种三萜皂苷和2种木脂素的含量(英文)[J]. J Chin Pharmaceut Sci,2014,23(12):866-872.
[21]杨鑫,丁怡,张东明.毛冬青中环烯醚萜苷类化合物的分离与鉴定[J].中国药物化学杂志,2007,17(3):173-177.
[22]杨燚,师帅,魏丹,等.毛冬青中环烯醚萜苷类化学成分的分离与鉴定[J].沈阳药科大学学报,2017,34(8):634-639.