正交试验法优选芪术颗粒提取工艺

Optimization of Extraction Process of Qizhu Granules by Orthogonal Test

摘要:

目的: 优选芪术颗粒的提取工艺,为该制剂的工业化生产提供参考。方法: 以黄芪甲苷、芍药苷提取量为综合评价指标,通过正交试验考察加水量、煎煮时间和煎煮次数对芪术颗粒水提工艺的影响。以特女贞苷和盐酸小檗碱提取量的综合评分为指标,通过正交试验考察溶剂用量、提取时间和提取次数对芪术颗粒醇提工艺的影响。采用HPLC-ELSD测定黄芪甲苷含量,流动相乙腈-水(34:66)。采用HPLC-DAD测定芍药苷、特女贞苷和盐酸小檗碱的含量,流动相分别为甲醇-0.05 mol·L^-1磷酸二氢钾溶液(30:70),甲醇-水(32:68)和乙腈-0.05 mol·L^-1磷酸二氢钾溶液(50:50),检测波长依次为230,224,345 nm。结果: 最佳水提取工艺为加12,10倍量水提取2次,每次2 h。最佳醇提工艺为加6倍量60%乙醇提取3次,每次2 h。结论: 优选的提取工艺稳定可行,适合推广于芪术颗粒的工业化生产。

Abstract:

Objective: To optimize extraction technology of Qizhu granules. Method: With contents of astragaloside and paeoniflorin as comprehensive evaluation index,orthogonal test was adopted to optimize water extracting technology.Taking composite score of extracting amounts of specnuezhenide and berberine hydrochloride as index,orthogonal test was adopted to optimize ethanol extraction process.The content of astragaloside was determined by HPLC-ELSD,mobile phase consisted of acetonitrile-water (34: 66).HPLC-DAD was employed to determine contents of paeoniflorin,specnuezhenide and berberine hydrochloride with mobile phases of methanol-0.05 mol·L^-1 potassium dihydrogen phosphate solution (30: 70),methanol-water (32: 68),0.05 mol·L^-1potassium dihydrogen phosphate solution-acetonitrile(50: 50) and detection wavelengths of 230,224,345 nm,respectively. Result: The best water extraction process was:extracted twice with 12,10 times the amount of water for 2 h per time.Optimum ethanol extraction process was as following:extracted thrice with 6 times the amount of 60% ethanol for 2 h each time. Conclusion: These optimized technologies are stable,feasible and suitable for standardized production of Qizhu granules.