基于响应曲面法的乳香有效部位提取纯化工艺优化研究

Optimization of extraction and purification process of effective components of Olibanum based on response surface method

目的对乳香中乳香酸类成分提取纯化工艺进行优选。方法采用UPLC-TQ/MS检测,以乳香中13个乳香酸(3-羰基甘遂-8,24-二烯-21-酸、3α-乙酰甘遂-7,24-二烯-21-酸、3-羟基甘遂烷-8,24-二烯-21-酸、乙酰11α-甲氧基-β-乳香酸、3α-羟基甘燧烷-7,24-二烯-21-酸、11-酮基乳香酸、3-O-乙酰基-α-乳香酸、3α-乙酰氧基-羊毛甾-8,24-二烯-21-酸、3β-乙酰氧基-5α-8,24-羊毛甾二烯-21-酸、3-乙酰基-11-酮基-β-乳香酸、3-乙酰基甲氧基甘遂-8,24-二烯-21-羧酸、α-乳香酸、β-乳香酸)的提取量及浸膏得率为评价指标,通过单因素及响应曲面法考察提取方法、提取溶剂、料液比、提取时间及提取次数对乳香提取工艺的影响;采用碱溶酸沉法纯化乳香提取物,并对纯化工艺参数进行单因素和正交试验考察,确定最佳纯化工艺。结果以95%乙醇20倍量回流提取4次,每次62min为最佳提取工艺;以碱液pH为12~13溶解,在0~4℃用酸液pH<2酸沉30 min为最佳纯化工艺,乳香酸类成分纯度可达73.87%。结论此优选的提取纯化工艺稳定可行,适用于乳香有效成分的提取纯化,为其物质基础研究提供科学依据。

Objective To optimize the extraction and purification process of the boswellic acids components in the frankincense.Methods The extraction amount and extract yield of 13 boswellic acids(3-oxotirucall-8,24-dien-21-oic acid,3α-acetoxy-tirucall-7,24-dien-21-oic acid,3-hydroxytirucall-8,24-dien-21-oic acid,acetyl 11α-methoxy-β-boswellic acid,3α-hydroxy tirucall-7,24-dien-21-oic acid,11-keto-boswellic acid,3-O-acetyl-α-boswellic acid,3α-acetyloxylanosta-8,24-dien-21-oic acid,3β-acetoxy-5α-lanosta-8,24-dien-21-oic acid,3-acetyl-11-keto-β-boswellic acid,3-acetyloxy-tirucall-8,24-dien-21-oic acid,α-boswellic acid,β-boswellic acid)in frankincense were detected by UPLC-TQ/MS,the extraction method was investigated by single factor and response surface,the extraction solvent,ratio of solid to liquid,extraction time and extraction times were investigated on the extraction process,and the extract was purified by alkali dissolving acid precipitation method and the purification process parameters were investigated by single factor and orthogonal test to determine the best purification process.Results The optimum condition for the extraction of the frankincense is that twenty times of 95%ethanol for four times reflux extraction and 62 min for each time.Optimum purification process was as following:Dissolve in lye pH 12—13,and the solution was precipitated at 0—4℃with pH<2 for 30 min.The purity of boswellic acids was 73.87%.Conclusion The optimized extraction and purification process is stable and feasible,which is suitable for the extraction and purification of effective fraction of frankincense and beneficial to give full play to the medicinal value of frankincense and provide scientific basis for material basis research of frankincense.