六堡茶中咖啡因加速溶剂萃取(ASE)的工艺研究
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摘要
本研究探讨了加速溶剂萃取(ASE)法提取六堡茶中咖啡因。采用快速溶剂萃取仪提取六堡茶中咖啡因,以乙醇为萃取溶剂,利用单因素试验考察乙醇浓度对提取率的影响,设置仪器压力为10MPa,选择萃取温度、萃取时间、循环次数等影响咖啡因得率的因素进行L_9(3~4)正交试验,以咖啡因得率为主要指标,考察ASE法最佳提取条件并与微波辅助提取法进行比较。结果显示ASE法提取六堡茶中咖啡因的最优化条件是以无水乙醇为溶剂,在温度120℃条件下静态萃取3次,每次10min;经ASE法提取,咖啡因的平均得率为20.374mg/g,其提取物经过C18固相萃取小柱处理不仅能除去六堡茶提取液中的大部分杂质,而且对咖啡因的含量几乎没有影响,经微波辅助法提取,咖啡因的平均得率为17.028mg/g。说明ASE法提取六堡茶中咖啡因,其提取率高于微波辅助提取法,且能保证提取物的质量。
This study investigated the extraction of caffeine from Liupao tea by accelerated solvent extraction(ASE). The caffeine from Liupao tea was extracted with an accelerated solvent extractor and ethanol as the extraction solvent. The effect of ethanol concentration on the extraction rate by single factor experiments, with the instrument pressure set to 10 MPa. The L_9(3~4) orthogonal test was carried out by selecting the factors affecting the caffeine yield such as extraction temperature, extraction time and cycle number. Taking the caffeine yield as the main index, the optimal extraction conditions for the ASE method were investigated and compared with the microwave-assisted extraction method.The results showed that the optimal extraction conditions for extracting caffeine from Liupao tea by ASE were: anhydrous ethanol as the solvent;static extraction 3 times at 120 ℃ with each lasting for 10 min. The average yield of caffeine for the ASE method was 20.374 mg/g, and the treatment with a C18 solid phase extraction column could only remove most of the impurities in the obtained Liupao tea extract with little effect on the content of caffeine. The average yield of caffeine was 17.028 mg/g for the microwave-assisted extraction. These results indicated that the extraction rate of caffeine from Liupao tea by ASE was higher than that by microwave-assisted extraction, and the quality of the obtained extract could be guaranteed.
This study investigated the extraction of caffeine from Liupao tea by accelerated solvent extraction(ASE). The caffeine from Liupao tea was extracted with an accelerated solvent extractor and ethanol as the extraction solvent. The effect of ethanol concentration on the extraction rate by single factor experiments, with the instrument pressure set to 10 MPa. The L_9(3~4) orthogonal test was carried out by selecting the factors affecting the caffeine yield such as extraction temperature, extraction time and cycle number. Taking the caffeine yield as the main index, the optimal extraction conditions for the ASE method were investigated and compared with the microwave-assisted extraction method.The results showed that the optimal extraction conditions for extracting caffeine from Liupao tea by ASE were: anhydrous ethanol as the solvent;static extraction 3 times at 120 ℃ with each lasting for 10 min. The average yield of caffeine for the ASE method was 20.374 mg/g, and the treatment with a C18 solid phase extraction column could only remove most of the impurities in the obtained Liupao tea extract with little effect on the content of caffeine. The average yield of caffeine was 17.028 mg/g for the microwave-assisted extraction. These results indicated that the extraction rate of caffeine from Liupao tea by ASE was higher than that by microwave-assisted extraction, and the quality of the obtained extract could be guaranteed.
引文
[1]滕翠琴,刘仲华,龚爱基,等.六堡茶对胰岛素抵抗3T3-L1脂肪细胞糖脂代谢的影响[J].茶叶科学,2014,34(3):230-238TENG Cui-qin,LIU Zhong-hua,GONG Ai-ji,et al.The effect of Liupao tea on the metabolism of insulin resistance3T3-L1 fat cells[J].Journal of Tea Science,2014,34(3):230-238
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[4]周芳,朱亚伟,位翠杰.正交试验法从茶叶中提取咖啡因的工艺研究[J].安徽农业科学,2015,43(19):274-275ZHOU Fang,ZHU Ya-wei,WEI Cui-jie.The process of extracting caffeine from tea leaves was studied by orthogonal test[J].Journal of Anhui Agricultural Sciences,2015,43(19):274-275
[5]刘静.ASE快速溶剂萃取-解决固体、半固体样品前处理的新技术[J].现代科学仪器,2002,12(3):59-60LIU Jing.The ASE fast solvent extraction-a new technique for treating solid and semi-solid samples[J].Modern Scientific Instruments,2002,12(3):59-60
[6]国务院标准委员会,食品安全国家标准,GB 5009:139-2014[S]The standards committee of the state council,National standards for food safety,GB 5009:139-2014[S]
[7]牟世芬,刘勇建.加速溶剂萃取的原理及应用[J].现代科学仪器,2001,45(3):18-20MOU Shi-fen,LIU Yong-jian.The principle and application of accelerated solvent extraction[J].Modern Scientific Instruments,2001,45(3):18-20
[8]韩亭亭,祁玥,王立宁.从茶叶中提取咖啡因的实验研究进展[J].广州化工,2017,45(1):28-31HAN Ting-ting,QI Yue,WANG Li-ning.Experimental research on extracting caffeine from tea[J].Guangzhou Chemicals,2017,45(1):28-31
[9]刘亚红,茶叶中咖啡因的提取[J].化工时刊,2016,30(2):29-32LIU Ya-hong.The extraction of caffeine from tea[J].Chemical Industry Times,2016,30(2):29-32
[2]杨巍,咖啡碱的药理作用与开发利用[J].茶叶科学技术,2006,21(4):9-10YANG Wei.The pharmacological action and exploitation of caffeine[J].Tea Science and Technology,2006,21(4):9-10
[3]黄飞,徐慧敏,王杰,等.Box-Behnken设计-效应面法优化离子液体提取废次茶叶中咖啡因工艺[J].天然产物研究与开发,2017,29:489-496HUANG Fei,XU Hui-min,WANG Jie,et al.Optimize the extraction of caffeine from ionic liquid by the Box-Behnken design-effect surface method[J].Natural Product Research and Development,2017,29:489-496
[4]周芳,朱亚伟,位翠杰.正交试验法从茶叶中提取咖啡因的工艺研究[J].安徽农业科学,2015,43(19):274-275ZHOU Fang,ZHU Ya-wei,WEI Cui-jie.The process of extracting caffeine from tea leaves was studied by orthogonal test[J].Journal of Anhui Agricultural Sciences,2015,43(19):274-275
[5]刘静.ASE快速溶剂萃取-解决固体、半固体样品前处理的新技术[J].现代科学仪器,2002,12(3):59-60LIU Jing.The ASE fast solvent extraction-a new technique for treating solid and semi-solid samples[J].Modern Scientific Instruments,2002,12(3):59-60
[6]国务院标准委员会,食品安全国家标准,GB 5009:139-2014[S]The standards committee of the state council,National standards for food safety,GB 5009:139-2014[S]
[7]牟世芬,刘勇建.加速溶剂萃取的原理及应用[J].现代科学仪器,2001,45(3):18-20MOU Shi-fen,LIU Yong-jian.The principle and application of accelerated solvent extraction[J].Modern Scientific Instruments,2001,45(3):18-20
[8]韩亭亭,祁玥,王立宁.从茶叶中提取咖啡因的实验研究进展[J].广州化工,2017,45(1):28-31HAN Ting-ting,QI Yue,WANG Li-ning.Experimental research on extracting caffeine from tea[J].Guangzhou Chemicals,2017,45(1):28-31
[9]刘亚红,茶叶中咖啡因的提取[J].化工时刊,2016,30(2):29-32LIU Ya-hong.The extraction of caffeine from tea[J].Chemical Industry Times,2016,30(2):29-32