| 昝珂,袁红,马双成,郑健,过立农.民族药材青阳参对照品的制备及质量标准提高研究[J].中国药事,2018,32(4):469-475 |
| 民族药材青阳参对照品的制备及质量标准提高研究 |
| Preparation of Reference Substance and Improvement of Its Quality Standard of Ethnic Medicine Cynanchi Otophylli Radix |
| 投稿时间：2017-10-23 |
| DOI：10.16153/j.1002-7777.2018.04.008 |
| 中文关键词: 青阳参 青阳参苷甲 白前 白薇 徐长卿 标准物质制备 含量测定 |
| 英文关键词: Cynanchi Otophylli Radix Otophylloside A Cynanchi Stauntonii Rhizoma et Radix Cynanchi Atrati Rhizoma et Radix Cynanchi Paniculati Rhizoma et Radix reference substance preparation determination of the content |
| 基金项目:国家食品药品监督管理总局药化注册司专项：“12种特色民族药材检验方法的示范性研究”. |
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| 中文摘要: |
| 目的：建立青阳参苷甲对照品的制备方法和含量测定，为质量标准的提高提供参考。方法：采用植物化学方法制备青阳参苷甲作为对照品，采用质谱、核磁共振等光谱法鉴定对照品的结构，采用面积归一化法测定了对照品含量，并建立高效液相色谱法测定青阳参及同属药材白前、白薇和徐长卿中青阳参苷甲的含量。采用Waters X Select C18色谱柱（4.6 mm×250 mm，5 μm），流动相为乙腈-水溶液（43：57），流速1.0 mL·min-1；检测波长223 nm；柱温30℃；进样量10 μL。结果：经过鉴定分离的青阳参苷甲纯度大于98%，可作为质量研究用对照品。青阳参苷甲质量浓度在5.62~224.8 μg·mL-1（r=0.9998，n=6）范围内线性关系良好，方法的平均回收率（n=6）为97.7%（RSD=1.4%）。白前、白薇和徐长卿中未检出青阳参苷甲，青阳参中青阳参苷甲含量在0.015%~0.070%。结论：青阳参苷甲是青阳参的特征成分，可作为该药材的定量指标。本文所建立的高效液相色谱法可作为青阳参药材质量标准中的含量测定方法。 |
| 英文摘要: |
| Objective: To establish a method to prepare and determine the content of otophylloside A as a reference substance for ethnic medicine Cynanchi Otophylli Radix so as to provide references for improving the quality standard. Methods: Otophylloside A isolated by phytochemical methods from Cynanchi Otophylli Radix was prepared as the reference substance. The structure of the reference substance was identifed by MS, NMR and other spectroscopic methods. The content of the reference substance was determined by area normalization method. HPLC method was established to detemine the content of otophylloside A in Cynanchi Otophylli Radix, Cynanchi Stauntonii Rhizoma et Radix, Cynanchi Atrati Rhizoma et Radix, and Cynanchi Paniculati Rhizoma et Radix. The separation was performed on a Waters XSelect C18 column (4.6 mm×250 mm, 5 μm) with acetonitrile-water (43:57) as mobile phase, the flow rate was 1.0 mL·min-1. The detection UV wavelength was at 223 nm, and the column temperature was 30℃. The injection volume was 10 μL. Results: The purity of isolated otophylloside A was more than 98% and could be used as a reference substance for quality research. There was a good linear relationship in the concentration range of otophylloside A from 5.62 to 224.8 μg·mL-1 (r=0.9998, n=6). The average recovery (n=6) of the method was 97.7% (RSD=1.4%). Otophylloside A was not detected in Cynanchi Stauntonii Rhizoma et Radix, Cynanchi Atrati Rhizoma et Radix, Cynanchi Paniculati Rhizoma et Radix. The content of otophylloside A in Cynanchi Otophylli Radix was 0.015%-0.070%. Conclusion: Otophylloside A is a characteristic component of Cynanchi Otophylli Radix and can be used as quantitative index of the ethnic medicine. The HPLC method established in the paper can be used for the determination of the content in the quality standard. |
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