基于HPLC特征图谱和多成分定量分析建立加味四妙颗粒的质量评价方法

Quality evaluation of Modified Simiao granule based on HPLC characteristic fingerprint and multicomponents simultaneous determination

目的建立加味四妙颗粒的对照特征图谱和多种成分进行定量分析方法,为本品质量控制和评价提供方法与依据。方法对20批加味四妙颗粒进行HPLC测定,采用中药色谱指纹图谱相似度评价系统(2012年版)生成加味四妙颗粒对照指纹图谱并进行相似度评价,将对照指纹图谱与各阴性供试品、混合对照品图谱进行匹配,对共有峰进行药味归属指认和多成分定量测定。结果各批次加味四妙颗粒样品与生成的对照指纹图谱相似度均在0.9以上;标定了19个共有峰,其中1、4、15号峰来源于川牛膝,2、6、10号峰来源于醋延胡索,3、16、18号峰来源于苍术,5、7号峰来源于大血藤,8、11号峰来源于薏苡仁,9、14、17号峰来源于黄柏,12、13、19号峰来源于甘草;指认了4、5、9、10、13、14、17、18、19共9个共有峰,即杯苋甾酮、红景天苷、木兰花碱、延胡索乙素、甘草苷、盐酸黄柏碱、盐酸小檗碱、苍术素、甘草酸铵,在相应的浓度范围内线性关系良好(r>0.9995),加样回收率在96.71%~102.92%之间,精密度、稳定性、重复性、加样回收率RSD值均小于3.0%。结论建立的加味四妙颗粒HPLC对照特征图谱和多指标成分定量测定方法,为加味四妙颗粒的质量控制和评价提供参考依据。

Objective To establish the HPLC characteristic fingerprint of Modified Simiao granule(MSG),identify the common peaksand determine the multi-components in MSG,thus to provide an approach and a basis for the quality control and evaluation in this product.Methods Twenty batches of MSG were determined by HPLC.The fingerprints of MSG were generated by the similarity evaluation system of chromatographic fingerprints of traditional Chinese medicine(2012 edition)and the similarity was evaluated.The fingerprints of the control group were matched with those of the negative samples and the mixed reference group.The common peaks were assigned and multi-components were determined.Results The similarity of fingerprints between the samples and the control fingerprints were above 0.9.Peaks 1,4,5 were from Cyathulae Radix,peaks 2,6,10 were from Corydalis Rhizoma,peaks 3,6,18 were from Atractylodis Rhizoma,peaks 5 and 7 were from Sargentodoxae Caulis,peaks 8 and 11 were from Coicis Semen,peaks 9,14,17 were from Phellodendri Chinensis Cortex,peaks 12,13,19 were from Glycyrrhizae Radix et Rhizoma.9 components[cyasterone(peak 4),rhodoglycoside(peak 5),magnoline(peak 9),tetrahydropalmatine(peak 10),liquiritin(peak 13),phellodendrine chloride(peak 14),berberine hydrochloride(peak 17),Rhizoma atractylodis(peak 18),ammonium glycyrrhizate(peak 19)]were identified and quantified.The linearity of the nine components were good(r>0.9995)in the corresponding concentration range.The recovery of the samples ranged from 96.71%to 102.92%.The RSD values of precision,stability,repeatability and recovery of the samples were all less than 3.0%.Conclusion This established method for the quantitative determination of MSG by HPLC characteristic fingerprint and multi-index composition provides a reference for he quality evaluation and quality control of MSG.