[关键词]
[摘要]
目的 基于一测多评法初步建立大黄地上部位提取物质量控制方法。方法 通过薄层色谱、指纹图谱主要色谱峰指认、紫外分光光度法和HPLC法对大黄地上部位提取物进行质量控制;建立芦荟大黄素、大黄酚、大黄素甲醚对大黄素的相对校正因子,利用其相对校正因子计算其量,实现一测多评。结果 薄层色谱供试品与对照品在相同位置显相同颜色斑点,提取物指纹图谱具有6个代表性色谱峰,其中5个已指认,总蒽醌在4.944~29.664 μg/mL线性良好(r = 0.999 0),一测多评法结果显示芦荟大黄素、大黄素、大黄酚及大黄素甲醚成分的平均回收率依次为97.08%、95.78%、100.60%、97.47%,其RSD依次为3.32%、2.42%、3.72%、2.67%。一测多评法与外标法比较没有显著性差异。结论 通过薄层色谱及指纹图谱可定性鉴别大黄地上部位提取物主要化学成分,紫外分光光度法可定量提取物中总蒽醌质量分数,一测多评法可定量提取物中芦荟大黄素、大黄素、大黄酚及大黄素甲醚的质量分数,该方法准确度高,重现性好,可用于大黄地上部位提取物质量控制。
[Key word]
[Abstract]
Objective To establish a method for the quality control of the extracts from the aerial parts of Rheum officinale (EARO) based on multi-assay depending on one determination (MDOD). Methods The quality control of EARO was carried out through the thin-layer chromatography(TLC), discrimination of chromatographic peak in fingerprint, ultraviolet spectrophotometric, and HPLC methods. The relative correction factors of aloe-emodin, chrysophanol, and physcione for detecting emodin were set up, the factors were used to measure their contents, and the method was adopted to the quality control of EARO. Results The experimental and control samples in TLC showed the same colored spots at the same position in EARO, five characteristic peaks among six were identified, and showed a good linear relationship at the range of 4.944—29.664 μg/mL (r = 0.999 0). The method of MDOD showed the recoveries of aloe-emodin, emodin, chrysophanol, and physcione were 97.08%, 95.78%, 100.60%, and 97.47%, and the RSD values were 3.32%, 2.42%, 3.72%, and 2.67%. There were no significant differences between MDOD method and external standard method. Conclusion TLC and fingerprint could be used to identify the chemical constituents in EARO, and ultraviolet spectrophotometry could be used to control the quantity of the total anthraquinone. The method of MDOD could be used to quantitatively control the contents of aloe-emodin, emodin, chrysophanol, and physcione, and the method is simple and accurate, which has a higher repeatability.
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[基金项目]
国家“十一五”科技支撑计划地方专项——灾区药材资源恢复重建与综合开发利用及示范(2009BAI84B00)