无糖型麦味地黄颗粒成型工艺的优化及有效成分含量测定

Forming process optimization of sugarless MaiweiDihuang granules and determination of active ingredient content

目的优化麦味地黄颗粒的成型工艺,并测定其有效成分含量。方法采用单因素试验结合Box-Behnken响应面法优选出麦味地黄颗粒的最佳成型工艺,并采用高效液相色谱(HPLC)法测定制剂中马钱苷、毛蕊花糖苷、丹皮酚的含量。结果麦味地黄颗粒的最佳成型工艺为牡丹皮、酒萸肉、山药粉碎成细粉,和糊精混合,药材细粉和糊精的混合药粉与稠膏配比为2︰1,乙醇体积分数为62%,乙醇用量为混合药粉的16%,颗粒干燥温度为60℃,麦味地黄颗粒制备贮存的临界相对湿度应控制在75%以下,马钱苷、毛蕊花糖苷、丹皮酚分别在0.676~67.600μg·ml^(-1)(r=0.9990)、0.806~80.600μg·ml^(-1)(r=0.9991)、1.094~109.400μg·ml^(-1)(r=0.9993)范围内线性关系良好,平均加样回收率为97.52%、97.11%、96.68%,RSD分别为1.23%、1.69%、1.98%。结论优化后的工艺稳定可靠,所制得的颗粒外观、粒度及流动性均较好,吸湿性小,可用于制备无糖型麦味地黄颗粒,HPLC法可用于麦味地黄颗粒中马钱苷、毛蕊花糖苷、丹皮酚等3种成分的含量测定。

Objective To optimize the forming process for MaiweiDihuang granules and to determine the content of its active components.Methods Single factor investigation test and Box-Behnken response surface methodology was used to optimize the forming process of MaiweiDihuang granules.The contents of loganin,verbascoside and paeonol were determined by HPLC.Results The optimal forming process is as follows:Moutan Cortex,Common Macrocarpium Fruit,and Chinese yam were crushed into fine powder and mixed with dextrin,and the rate of medicinal material powder to Dextrin was 2︰1,the volume fraction of ethanol was 62%,the dosage of ethanol was 16%of mixed fine powder,and the drying temperature of granules was 60℃and the preparation and storage of MaiweiDihuang granules should be controlled under 75%of critical relative humidity.The linear range of loganin,verbascoside and paeonol was performed well when they were within the range of 0.676~67.600μg ml^(-1)(r=0.9990),0.806-80.600μg ml^(-1)(r=0.9991),and 1.094~109.400μg ml^(-1)(r=0.9993).The average sample recovery were 97.52%,97.11%,and 96.68%.The average relative standard deviation of them were 1.23%,1.69%,and 1.98%.Conclusions The optimized process is stable and reliable.The prepared granules have good appearance,particle size and fluidity,and low hygroscopicity.This stable and feasible method can be used to prepare sugarless MaiweiDihuang granules.HPLC method can be used for the content determination of loganin,verbascoside and paeonol of MaiweiDihuang granules.