中国中药杂志

2019, v.44(07) 1371-1380

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基于特征图谱和多成分含量测定的茯苓质量评价研究
Quality evaluation of Poria based on specific chromatogram and quantitative analysis of multicomponents

田双双;刘晓谦;冯伟红;张启伟;闫利华;王智民;高陆;
TIAN Shuang-shuang;LIU Xiao-qian;FENG Wei-hong;ZHANG Qi-wei;YAN Li-hua;WANG Zhi-min;GAO Lu;Henan University of Chinese Medicine;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines, Institute of Chinese Materia Medica, China Academy of Chinese Medical Sciences;Xiuzheng Pharmaceutical Group Co., Ltd.;

摘要(Abstract):

该文建立了茯苓三萜类成分的HPLC特征图谱,并同时测定16α-羟基松苓新酸、茯苓新酸B、去氢土莫酸、茯苓新酸A、猪苓酸C、茯苓新酸AM、3-O-乙酰-16α-羟基松苓新酸、去氢茯苓酸、茯苓酸、松苓新酸10个三萜类成分的含量。采用Welch Ultimate XB C_(18)色谱柱(4.6 mm×250 mm,5μm);流动相为乙腈(含3%四氢呋喃)(A)和0.1%甲酸水溶液(B),梯度洗脱,流速1.0 mL·min(-1);柱温30℃;检测波长201,243 nm;进样量20μL。采用SPSS 22.0及GraphPad Prism 7.0对茯苓药材与饮片、不同产地茯苓样品数据进行分析。结果显示,所建立的特征图谱专属性强,10个待测成分能够达到良好分离,在考察的范围内线性关系良好(r≥0.999 6),平均回收率98.53%~103.8%,RSD 1.7%~2.7%。该方法重复性好,专属性强,可用于茯苓的鉴别及质量控制。研究结果表明,茯苓中10个三萜类成分之间具有正相关;产地收集的药材中各成分的含量均高于市售饮片;湖北、云南产茯苓10个成分的总含量略高于安徽,但安徽产茯苓中各成分的含量波动范围较小。
HPLC specific chromatograms of Poria were established, and the concentrations of 10 triterpenoids(16α-hydroxydehydrotrametenolic acid, poricoic acid B, dehydrotumulosic acid, poricoic acid A, polyporenic acid C, poricoic acid AM, 3-O-acetyl-16α-hydroxydehydrotrametenolic acid, dehydropachymic acid, pachymic acid, and dehydrotrametenolic acid) were simultaneously determined. Chromatographic analysis was conducted on a Welch Ultimate XB C_(18) column(4.6 mm × 250 mm,5 μm). Acetonitrile solution(contain 3% tetrahydrofuran)(A) and 0.1% formic acid aqueous solution(B) were used as the mobile phase with gradient elution at a flow rate of 1.0 mL·min(-1);柱温30℃;检测波长201,243 nm;进样量20μL。采用SPSS 22.0及GraphPad Prism 7.0对茯苓药材与饮片、不同产地茯苓样品数据进行分析。结果显示,所建立的特征图谱专属性强,10个待测成分能够达到良好分离,在考察的范围内线性关系良好(r≥0.999 6),平均回收率98.53%~103.8%,RSD 1.7%~2.7%。该方法重复性好,专属性强,可用于茯苓的鉴别及质量控制。研究结果表明,茯苓中10个三萜类成分之间具有正相关;产地收集的药材中各成分的含量均高于市售饮片;湖北、云南产茯苓10个成分的总含量略高于安徽,但安徽产茯苓中各成分的含量波动范围较小。
HPLC specific chromatograms of Poria were established, and the concentrations of 10 triterpenoids(16α-hydroxydehydrotrametenolic acid, poricoic acid B, dehydrotumulosic acid, poricoic acid A, polyporenic acid C, poricoic acid AM, 3-O-acetyl-16α-hydroxydehydrotrametenolic acid, dehydropachymic acid, pachymic acid, and dehydrotrametenolic acid) were simultaneously determined. Chromatographic analysis was conducted on a Welch Ultimate XB C_(18) column(4.6 mm × 250 mm,5 μm). Acetonitrile solution(contain 3% tetrahydrofuran)(A) and 0.1% formic acid aqueous solution(B) were used as the mobile phase with gradient elution at a flow rate of 1.0 mL·min(-1). The column temperature was 30 ℃ and the injection volume was 20 μL. The experimental data were analyzed by the SPSS 22.0 and GraphPad Prism 7.0. The established triterpenoids fingerprints were specific, and the 10 components were well separated and showed good linearity(r≥0.999 6) within the concentration ranges tested. The mean recoveries were between 98.53%-103.8%(RSD 1.7%-2.7%). The method was specific and repeatable, and could be used for identification and quality evaluation of Poria. The results showed that the contents of 10 triterpenoids were positively correlated with each other. The contents of 10 triterpenoids of samples collected from producing areas were higher than that collected from markets. The total contents of 10 triterpenoids of samples collected from Hubei and Yunnan province were slightly higher than that from Anhui province, but the contents of samples from Anhui province were varied in smaller ranges.

关键词(KeyWords): 茯苓;三萜;高效液相色谱;特征图谱;含量测定
Poria cocos;triterpenoids;HPLC;specific chromatograms;contents determination

Abstract:

Keywords:

基金项目(Foundation): 国家中药标准化项目(ZYBZH-C-JL-24)

作者(Authors): 田双双;刘晓谦;冯伟红;张启伟;闫利华;王智民;高陆;
TIAN Shuang-shuang;LIU Xiao-qian;FENG Wei-hong;ZHANG Qi-wei;YAN Li-hua;WANG Zhi-min;GAO Lu;Henan University of Chinese Medicine;National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines, Institute of Chinese Materia Medica, China Academy of Chinese Medical Sciences;Xiuzheng Pharmaceutical Group Co., Ltd.;

DOI: 10.19540/j.cnki.cjcmm.20181220.005

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