归芪益元膏提取工艺优化及质量控制方法研究

Study on Extraction Process Optimization and Quality Control Method of Guiqi Yiyuan Decoction

关键词:  提取工艺  毛蕊异黄酮葡萄糖苷  质量标准  相对密度

Key words:  extraction process  glucoside of calycosin  quality standard  relative density

摘要:

目的 优化归芪益元膏的提取工艺并建立其质量控制方法。方法 采用L₉(3⁴)正交试验法，以出膏率、总多糖含量及正丁醇浸出物含量的综合评价为指标，优化归芪益元膏提取工艺；采用薄层色谱(TLC)法，对煎膏剂中的黄芪、当归、枸杞子、人参进行定性鉴别；采用HPLC测定方中君药黄芪的主要活性成分毛蕊异黄酮葡萄糖苷的含量；参照中国药典2020年版检查其相对密度、不溶物和装量差异，建立其质量控制方法。结果 最佳工艺为加水量12倍，提取时间4 h，提取2次；TLC鉴定结果显示色谱图斑点清晰，分离度良好且专属性强；毛蕊异黄酮葡萄糖苷在0.089 6~1.344 0 µg内线性关系良好(r²=0.999 4)，平均回收率为99.51%，RSD为2.59%(n=9)；煎膏相对密度为1.39，不溶物和装量差异符合中国药典2020年版规定。结论 优选的水提工艺科学合理，质量标准有效可控，可用于归芪益元膏的质量控制。

Abstract:

OBJECTIVE To optimize the extraction process of Guiqi Yiyuan decoction and establish its quality control method. METHODS L₉(3⁴) orthogonal test was used to optimize the extraction process of Guiqi Yiyuan decoction by using index as comprehensive evaluation of the extraction rate, total polysaccharide content and n-butanol extract content. Thin layer chromatography(TLC) was used to identify Astragali Radix, Angelicae Sinensis Radix, Lycii Fructus and Ginseng Radix et Rhizoma in the decoction. The content of glucoside of calycosin as the main active ingredient of Astragali Radix was determined by HPLC. The differences in relative density, insoluble matter and loading amount were checked according to the Chinese Pharmacopoeia 2020 edition, and the quality control method was established. RESULTS The optimum process was 12 times water, 4 h extraction time and 2 times extraction. TLC identification results showed that the chromatograms had clear spots, good separation and strong specificity. The linear range of calycosin glucoside was 0.089 6-1.344 0 µg(r²=0.999 4), the average recovery was 99.51%, RSD was 2.59%(n=9). The relative density of decoction was 1.39, and the difference of insoluble matter and loading amount was in accordance with the provisions of Chinese Pharmacopoeia 2020 edition. CONCLUSION The optimized water extraction process is scientific and reasonable, and the quality standard is effective and controllable, which can be used for the quality control of Guiqi Yiyuan decoction.