中国中药杂志

2019, v.44(04) 730-739

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以脱水穿心莲内酯为内参物建立中药穿心莲“一测多评”质量控制方法
Establishment of QAMS method with dehydroandrographolide as internal reference substance for quality control of Andrographis Herba

陈两绵;高慧敏;胡雪花;朱晶晶;冯伟红;闫利华;刘晓谦;张永欣;王智民;
CHEN Liang-mian;GAO Hui-min;HU Xue-hua;ZHU Jing-jing;FENG Wei-hong;YAN Li-hua;LIU Xiao-qian;ZHANG Yong-xin;WANG Zhi-min;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicine,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;Yunnan University of Traditional Chinese Medicine;

摘要(Abstract):

针对中药穿心莲现有研究中,以穿心莲内酯为内参物建立的"一测多评"(QAMS)方法存在色谱分离的分离度不佳,相对校正因子的耐用性不强及含量测定结果的准确度不高等问题,该研究通过色谱条件的优化和方法学的系统考察,首次采用脱水穿心莲内酯为内参物,建立同步测定穿心莲中穿心莲内酯(A)、新穿心莲内酯(B)、14-去氧穿心莲内酯(C)和脱水穿心莲内酯(S)等4种二萜内酯的"一测多评"质量控制方法。在当前HPLC色谱条件下,待测成分分离度良好(R>1. 5),方法学考察符合定量分析的要求。该法确立的相对校正因子(RCFs)分别为:fA/S=0. 65,fB/S=0. 54,fC/S=0. 78,相对校正因子在3种品牌HPLC仪、5种品牌C18柱、不同流速(0. 9,1. 0,1. 1 m L·min~(-1))和不同柱温(25,30,35℃)下的RSD分别为1. 3%~5. 1%,0. 25%~0. 33%,0. 070%~0. 15%,0. 070%~0. 22%,表明相对校正因子的耐用性良好。采用相对保留值法对待测成分的色谱峰进行定位,其相对保留值分别为:rA/S=0. 44,rB/S=0. 86,rC/S=0. 97,相对保留值在不同仪器不同色谱柱下的RSD为0. 030%~1. 6%,表明待测成分的色谱峰定位准确。分别采用QAMS法和外标法(ESM)对6批穿心莲药材和18批穿心莲饮片中的上述4种成分进行含量测定,2种方法所得结果的相对误差均<2. 0%,无显著性差异,表明当前QAMS法的准确度良好。因此,该研究以脱水穿心莲内酯为内参物建立了4种二萜内酯类成分同步测定的"一测多评"方法,该法准确度高,耐用性强,能有效控制穿心莲的内在质量,可以为穿心莲行业标准的制订及药典标准的完善提供技术依据。
To solve the problems of the poor resolution of chromatographic separation,the weak durability of the relative correction factors,and the low accuracy of content determination results in the quantitative analysis of multi-components by single-marker( QAMS) method with andrographolide as the internal reference substance in the existing research of Andrographis Herba,a new QAMS method using dehydroandrographolide as the internal reference substance was established for the first time in this study. This new method can be used to simultaneously determine four diterpene lactones,including andrographolide( A),neoandrographolide( B),14-deoxyandrographolide( C),and dehydroandrographolide( S) through the optimization of chromatographic conditions and systematic investigation of methodology. At the present HPLC chromatographic conditions,four components could be well separated( R > 1. 5),and the methodology validations could satisfy the requirement of quantitative analysis. The relative correction factors( RCFs) of fA/S,fB/S,fC/S were determined as 0. 65,0. 54,0. 78,respectively. The relative standard deviations( RSDs) of their RCFs ranged between 1. 3%-5. 1%,0. 25%-0. 33%,0. 070%-0. 15%,0. 070%-0. 22%,respectively with three brands of HPLC instruments,five brands of C18 column,different flow rates( 0. 9,1. 0,1. 1 m L·min~(-1)),and different column temperatures( 25,30,35 ℃),indicating good durability of the RCFs. The relative retention value( RRV) method was used to locate the chromatographic peak of the components to be determined.The RRVs of rA/S,rB/S,and rC/Swere 0. 44,0. 86,0. 97,respectively. The RSDs of the RRVs ranged between 0. 030%-1. 6% with different HPLC instruments and columns,showing accurate peak location. The present QAMS method and the external standard method( ESM)were both used to determine the contents of four diterpene lactones from Andrographis Herba( 6 batches of medicinal materials and 18 batches of cut crude drugs). The relative errors of the determined content results between two methods were less than 2. 0%. It demonstrated that there was no significant difference in content results between these two methods,indicating good accuracy of the present QAMS method. Therefore,in this study,an accurate and highly durable QAMS method using dehydroandrographolide as the internal reference substance was established for simultaneous determination of four diterpene lactones. This method could be used to effectively control the quality of Andrographis Herba and provide technical basis for the formulation of traditional Chinese medicine industry standard and improvement of the Chinese Pharmacopoeia standard of Andrographis Herba.

关键词(KeyWords): 穿心莲;一测多评法;相对校正因子;中药质量控制;二萜内酯
Andrographis Herba;QAMS method;relative correction factor;quality control of traditional Chinese medicine;diterpene lactones

Abstract:

Keywords:

基金项目(Foundation): 国家中药标准化项目(ZYBZH-Y-GD-12);; 国家药典委员会课题(2018Z005)

作者(Author): 陈两绵;高慧敏;胡雪花;朱晶晶;冯伟红;闫利华;刘晓谦;张永欣;王智民;
CHEN Liang-mian;GAO Hui-min;HU Xue-hua;ZHU Jing-jing;FENG Wei-hong;YAN Li-hua;LIU Xiao-qian;ZHANG Yong-xin;WANG Zhi-min;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicine,Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences;Yunnan University of Traditional Chinese Medicine;

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