甘草超滤液中甘草酸的络合萃取研究
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摘要
以甘草酸的单次萃取率及甘草酸与甘草苷的分离率为指标,以0.2 g/mL的甘草超滤液为研究对象,在单因素实验基础上,应用析因实验考察络合萃取剂组成变化对甘草超滤液中甘草酸萃取效果的影响,优选出适合甘草酸分离的络合萃取剂及方法。结果表明:15%三烷基氧磷(TRPO)+85%磺化煤油对甘草超滤液中甘草苷的单次萃取率为99.59%,甘草苷与甘草酸的分离率为91.31%; 6%TRPO+50%磷酸三丁酯(TBP)+44%磺化煤油对甘草酸的单次萃取率为32.98%±0.04%。得到先用15%TRPO+85%磺化煤油络合萃取超滤液中的甘草苷,再以6%TRPO+50%TBP+44%磺化煤油为萃取剂,萃取萃余水相中甘草酸的两步络合萃取法。该两步络合萃取法既能得到甘草酸,同时还可收集到副产品甘草苷。
The single extraction rate of glycyrrhizic acid and the separation rate of glycyrrhizic acid and liquorice were used as indexes,the Glycyrrhiza uralensis ultrafiltration liquid with a concentration of 0.2 g/mL was taken as the research object.Based on the single factor experiments,the factorial experiment was employed to investigate the influence on the extracting effect of glycyrrhizic acid in glycyrrhiza ultrafiltration liquid by changing the composition of complexing extractants,to screen out a complexing extractant and method suitable for separation of glycyrrhizic acid.The results showed that the single extraction rate of 15% TRPO + 85% sulfonated kerosene for liquiritin of glycyrrhiza ultrafiltration liquid was 99.59%,the separation rate of liquiritin and glycyrrhizic acid was 91.31%.The single extraction rate of 6% TRPO + 50% TBP + 44% sulfonated kerosene for glycyrrhizic acid was 32.98% ± 0.04%.The preparation of glycyrrhizic acid by two step complexation extraction was obtained,it was that 15% TRPO + 85% sulfonated kerosene was used to extract glycyrrhizin in the ultrafiltration fluid first,and then 6%TRPO + 50% TBP + 44% sulfonated kerosene as the extractant to extract glycyrrhizic acid from the extracted water phase.The two step complexation extraction method could obtain glycyrrhizic acid and collect by-product liquiritin.
The single extraction rate of glycyrrhizic acid and the separation rate of glycyrrhizic acid and liquorice were used as indexes,the Glycyrrhiza uralensis ultrafiltration liquid with a concentration of 0.2 g/mL was taken as the research object.Based on the single factor experiments,the factorial experiment was employed to investigate the influence on the extracting effect of glycyrrhizic acid in glycyrrhiza ultrafiltration liquid by changing the composition of complexing extractants,to screen out a complexing extractant and method suitable for separation of glycyrrhizic acid.The results showed that the single extraction rate of 15% TRPO + 85% sulfonated kerosene for liquiritin of glycyrrhiza ultrafiltration liquid was 99.59%,the separation rate of liquiritin and glycyrrhizic acid was 91.31%.The single extraction rate of 6% TRPO + 50% TBP + 44% sulfonated kerosene for glycyrrhizic acid was 32.98% ± 0.04%.The preparation of glycyrrhizic acid by two step complexation extraction was obtained,it was that 15% TRPO + 85% sulfonated kerosene was used to extract glycyrrhizin in the ultrafiltration fluid first,and then 6%TRPO + 50% TBP + 44% sulfonated kerosene as the extractant to extract glycyrrhizic acid from the extracted water phase.The two step complexation extraction method could obtain glycyrrhizic acid and collect by-product liquiritin.
引文
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[4]李玉山.甘草酸提取纯化工艺的研究进展[J].化学试剂,2016,38(5):428-432.
[5]李海华,青梅,于娟,等.甘草的研究进展[J].内蒙古医科大学学报,2015(2):199-204.
[6]田庆来,谢渝春,张波,等.溶剂萃取法分离水溶性甘草黄酮[J].过程工程学报,2007,7(3):496-500.
[7]朱应怀,刘晓霞,王继龙,等.基于陶瓷膜超滤技术的甘草酸和甘草苷同步提取纯化工艺研究[J].中草药,2016,47(23):4173-4178.
[8]国家药典委员会.中国药典[S].一部.中国医药科技出版社,2015.
[9]常志显.三烷基氧磷络合萃取氨基苯酚稀溶液的研究[D].开封:河南大学,2007.
[10]杨琳,梁政.液-液水力旋流器油水乳化机理研究[J].石油机械,2007,35(12):8-11.
[11]戴猷元,秦炜,张瑾,等.有机物络合萃取化学[M].北京:化学工业出版社,2015(7):18-22.
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[13]徐晨.醋酸稀溶液络合萃取过程研究[D].南京:南京工业大学,2004.