响应面法优化暗紫贝母流浸膏提取工艺及其质量评价

Optimization of the extraction process of Fritillaria unibracteata fluidextract by response surface methodology and its quality evaluation

优化暗紫贝母流浸膏提取工艺,评价暗紫贝母流浸膏质量。以总生物碱含量、贝母辛含量、贝母素甲、贝母素乙和西贝母碱三碱含量之和、浸膏得率的综合评分作为评价指标,采用单因素实验确定乙醇体积分数、乙醇用量、浸润时间、渗漉速度4个因素对暗紫贝母流浸膏提取的影响;利用Box-Benhnken响应面法确定并验证暗紫贝母流浸膏的最优渗漉提取工艺条件;采用薄层色谱法对暗紫贝母药材进行定性鉴别,并对其水分、灰分及浸出物进行检查;采用薄层色谱建立暗紫贝母流浸膏中贝母辛、贝母素乙的定性鉴别方法,并对其乙醇量和重金属进行检查。结果表明暗紫贝母流浸膏的最佳提取工艺为:乙醇体积分数为70%,乙醇用量为18倍,浸润时间为39 h,渗漉速度为3 mL/(kg·min),在此条件下暗紫贝母流浸膏综合评分为(89.97±1.90)%。药材和流浸膏TLC结果斑点清晰,分离度好,药材水分不超过15%、灰分不超过5.0%及浸出物大于9.0%,暗紫贝母流浸膏的乙醇量和重金属检查均符合《中华人民共和国药典》流浸膏制剂规定。本研究优化的暗紫贝母流浸膏提取工艺稳定可行,为暗紫贝母开发利用提供参考。

This study aims to optimise the extraction process and evaluate the quality of Fritillaria unibracteata fluid extract(FUFE).The comprehensive score of total alkaloid content,the content of peimisine,the sum of the three alkaloid contents of peimine,peiminine and sipeimine,and the extraction rate were used as the evaluation indexes,and the single factor experiment were used to determine the effects of the volume fraction of ethanol,the amount of ethanol,the infiltration time,and the percolation speed on the extraction of FUFE;The Box-Benhnken response surface method was used to determine and verify the optimal percolation extraction process conditions of FUFE;the qualitative identification of F.unibracteata by thin-layer chromatography(TLC),and the examination of its moisture,ash and leachate;the establishment of a TLC method for the qualitative identification of peimisine and peiminine in the FUFE,and the examination of its ethanol amount and heavy metals.The results showed that the optimal extraction process for FUFE ware as flows:ethanol volume fraction 70%,ethanol dosage 18 times,infiltration time 39 h,and percolation rate 3 mL/(kg·min),and the comprehensive score of FUFE under these conditions was(89.97±1.90)%.The TLC results of the herbs and the fluid extract were clear spots with good separation,the moisture of the herbs was not more than 15%,the ash was not more than 5.0%and the leachate was more than 9.0%,and the amount of ethanol and the examination of heavy metals of FUFE complied with the provisions of the Chinese Pharmacopoeia for fluid extract preparation.The optimised extraction process of FUFE is stable and feasible,and provides a reference for the development and utilization of F.unibracteata.