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大孔吸附树脂分离纯化牛蒡叶绿原酸的工艺研究

2020-03-31袁晓庆李莉刘言娟王振

安徽农业科学 2020年4期

袁晓庆 李莉 刘言娟 王振

摘要[目的]建立大孔吸附樹脂分离纯化牛蒡叶中绿原酸的工艺。[方法]通过单因素试验研究提取液种类、浓度、pH、提取温度、料液比以及提取时间等参数对绿原酸提取率的影响,确定最佳提取工艺;以大孔吸附树脂对牛蒡叶中绿原酸的分离效率为评价指标,通过静态和动态吸附/解吸附试验优化分离纯化工艺。[结果]pH=1的蒸馏水为提取溶剂,料液比1∶20(g∶mL)、提取温度80 ℃、回流1 h时对牛蒡叶中绿原酸的提取效果最佳,平均提取率为1.82%;考察了6种大孔吸附树脂对牛蒡叶绿原酸的分离纯化性能,以吸附/解吸附性能为评价指标,确定了LX-218为最佳大孔吸附树脂。LX-218型MAR分离纯化牛蒡叶绿原酸的最佳工艺条件为:上样量为30 BV(树脂床体积),上样浓度为0.7倍提取原液浓度(相当于原生药),上样液pH=3,以4 BV/h流速吸附,5 BV pH=5的60%乙醇以5 BV/h的流速解吸附。在优化的工艺条件下,牛蒡叶绿原酸得率为84.41%,纯度为55.26%。[结论]LX-218型大孔吸附树脂对牛蒡叶绿原酸有较好的吸附容量和解吸附率,优化的生产工艺条件适用于牛蒡叶绿原酸的工业化生产。

关键词牛蒡叶;大孔吸附树脂;绿原酸;分离纯化;工艺优化

中图分类号R284.2文献标识码A

文章编号0517-6611(2020)04-0168-07

doi:10.3969/j.issn.0517-6611.2020.04.049

开放科学(资源服务)标识码(OSID):

Study on the Technology of Separation and Purification of Chlorogenic Acid from Burdock Leaves by Macroporous Adsorption Resin

YUAN Xiao-qing,LI Li,LIU Yan-juan et al(Linyi University,Linyi,Shandong 276000)

Abstract[Objective]To establish the optimum technological conditions for the separation and purification of chlorogenic acid from burdock leaves by macroporous adsorption resin(MAR).[Method]The optimum extraction process was obtained by studying the effects of extractant type,concentration,pH,extraction temperature,ratio of solid-liquid ratio and extraction time with single factor experiment.Based on separation efficiency of chlorogenic acid from burdock leaves,the optimal separation and purification processes were obtained by static and dynamic adsorption/desorption experiments.[Result]The optimum extraction process as follows:the extractant was distilled water with pH=1,the ratio of solid-liquid ratio was 1:20(g:mL),the extraction temperature was 80 °C,the reflux time was 1 h.The average extraction rate was 1.82% with the above extraction process.The separation and purification performance of six kinds of macroporous adsorption resins for burdock chlorogenic acid were investigated.Taking adsorption / desorption performance as the evaluation index,LX-218 was determined as the best macroporous adsorption resin.The optimal process conditions on LX-218 MAR for the separation and purification of burdock chlorophyllic acid as follows:the loading amount was 30 BV(resin bed volume),the loading concentration was 0.7 times the concentration of the extracted stock solution(equivalent to raw material),and the loading solution pH=3,adsorption at 4 BV/h flow rate,respectively.For the desorption process,chlorogenic acid loaded MAR column was desorbed by 5 BV ethanol-aqueous solution(60∶40,V∶V) with pH value of 5 at flow rate of 5 BV/h.Under the optimal conditions,the yield of chlorogenic acid from burdock leaves and purity were 84.41% and 55.26%,respectively.[Conclusion]LX-218 macroporous adsorption resin has good adsorption and desorption performance for chlorogenic acid.The optimized technique is suitable for the industrial production of chlorogenic acid from burdock leaves.

Key wordsBurdock leaves;Macroporous adsorption resin;Chlorogenic acid;Separation and purification;Process optimization

牛蒡又名大力子、恶实、牛蒡子,属于菊科类植物,近年来作为保健型蔬菜受到人们的青睐。它全身是宝,其子、根均可入药,富含糖、纤维素、蛋白质、钙、铁等人体所需的多种营养物质和矿物质等[1-2]。我国是牛蒡生产大国,仅临沂市兰陵县的庄坞、层山、二庙等乡镇,种植面积达0.67万hm2以上,县外发展种植基地0.80万hm2以上,年总产量约70万t,占全国牛蒡产量的50%以上。……

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