| 冯欣,鲁晓光,仲格嘉,看召本.松石散鉴别及含量测定方法研究[J].中国药事,2021,35(3):315-322 |
| 松石散鉴别及含量测定方法研究 |
| On Identification and Determination Methods of the Tibetan Medicine Songshisan |
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| DOI：10.16153/j.1002-7777.2021.03.011 |
| 中文关键词: 松石散 质量标准 显微鉴别 薄层色谱鉴别 气相色谱法 龙脑 丁香酚 麝香酮 |
| 英文关键词: Songshisan quality standard microscopic identification TLC GC borneol eugenol muscone |
| 基金项目:重大新药创制：藏医治疗肝病的创新药物研究(编号 2014ZX09301308-003) |
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| 中文摘要: |
| 目的：建立藏药松石散的定性定量检测方法，完善质控标准，提升其质量控制水平。方法：采用显微鉴别方法对制剂中丁香、檀香、波棱瓜子进行鉴别。选用薄层色谱法(TLC)对制剂中丁香、 熊胆、波棱瓜子进行定性鉴别。选择气相色谱法(GC)测定龙脑、丁香酚和麝香酮的含量：DB-WAX 毛细管色谱柱(30 m×0.32 mm×0.25μm)；程序升温；载气为氮气；流速1.0 mL·min-1；空气流速 450 mL·min-1；氢气流速45 mL·min-1；进样量1 μL；分流进样，分流比20︰1；FID检测器，温度 250 ℃；进样口温度210 ℃。结果：丁香、檀香、波棱瓜子的显微鉴别特征显著；丁香、波棱瓜子、熊胆的薄层色谱斑点清楚，阴性对照无干扰；GC含量测定法中，龙脑、丁香酚、麝香酮分别在0.1958~ 3.9172μg、0.0306~0.6124μg、0.0050~0.0992μg内线性关系良好，相关系数分别为0.9958、0.9944、 0.9922，平均回收率分别为99.79%、98.66%、94.13%，RSD分别为1.86%、1.43%、1.91%。结论：所建方法具有较强的专属性，准确度高，为质量标准的完善提供了依据。 |
| 英文摘要: |
| Objective: To improve the quality standard of Tibetan medicine Songshisan, enhance its quality control level and establish the qualitative and quantitative detection methods. Methods: The microscopic identification method was used to identify Eugenia caryophyllata, Santalum album and herpetospermum caudigerum in the preparation. Thin layer chromatography (TLC) was used for qualitative identification of eugenia caryophyllata, herpetospermum caudigerum and bear gall in the preparation. Gas chromatography (GC) was selected for the determination of borneol, eugenol and muscone. The GC system proceeded as following: DB-WAX capillary column was 30 m×0.32 mm×0.25μm. The column temperature was raised by program. The carries gas was nitrogen and the flow rate of carries gas was 1.0 mL·min-1. The air flow rate was 450 mL·min-1. The hydrogen flow rate was 45 mL·min-1. The injection volume was 1 μL. Split-flow injection with a split ratio of 20∶1. The temperature of FID detector was at 250 ℃. The temperature of the inlet port was 210 ℃. Results:Microscopic identification features of Eugenia caryophyllata, Santalum album and herpetospermum caudigerum were significant. The TLC spots of eugenia caryophyllata, herpetospermum caudigerum and bear gall were clear, and the negative control had no interference. According to the GC analysis, the calibration curves were linear within the range of 0.1958-3.9172 μg for borneol, 0.0306-0.6124 μg for eugenol, 0.0050-0.0992 μg for muscone. Correlation coefficient were 0.9958, 0.9944 and 0.9922, respectively. The average recoveries were 99.79%, 98.66% and 94.13%, respectively. RSD were 1.86%, 1.43% and 1.91%, respectively. Conclusion: The established method has strong specificity and high accuracy, which provides a basis for the improvement of quality standards. |
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