均匀设计法优化甜茶叶中总黄酮提取工艺
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摘要
为优化优选纤维素酶-乙醇提取法、乙醇热回流提取法和超声波-乙醇提取法对甜茶叶中总黄酮的提取工艺,采用单因素和均匀设计法相结合进行试验,以甜茶叶中总黄酮的提取得率为指标,对均匀设计实验数据进行回归分析和二次多项式逐步回归分析等。试验结果表明,纤维素酶-乙醇提取法的较优工艺条件:酶添加量为4.3 mg(0.86%)、酶解液p H值为5.4、酶解温度为42℃、酶解时间为65 min,此条件下甜茶总黄酮提取得率最大为10.89%;乙醇热回流提取法的较优工艺条件:乙醇浓度为63%、料液比为1∶58(g/mL)、提取温度为60℃、提取时间为120 min,此条件下甜茶总黄酮提取得率最大为11.53%;超声波-乙醇提取法的较优工艺条件:乙醇浓度为68.9%、料液比为1∶30(g/mL)、超声波功率为73.9 W、提取温度为62.2℃、提取时间为67.7 min,此条件下甜茶总黄酮提取得率最大为12.23%。3种提取方法比较,超声波-乙醇提取法提取得率平均为12.23%>乙醇热回流提取得率平均为11.53%>纤维素酶-乙醇提取法提取得率平均为10.89%,3种提取方法对甜茶叶总黄酮提取得率的影响差异达到了高度(十分)显著水平。
In order to optimize the extraction process of total flavonoids in sweet tea,the extraction process of cellulase ethanol extraction,ethanol hot reflux extraction and ultrasonic ethanol extraction was optimized. The experiment was carried out by the combination of single factor and uniform design method. The extraction rate of total flavonoids in sweet tea was taken as the index,and the experimental data of uniform design were regressed analysis and two polynomial stepwise regression analysis. The experimental results showed that the optimum technological conditions for the extraction of cellulase and ethanol were enzyme addition was 4.3 mg(0.86 %),the pH value of the hydrolysate was 5.4,the hydrolysis temperature was 42 ℃,and the enzymolysis time was65 min,under this conditions the maximum extraction yield of the total flavonoids was 10.89 %. The optimum technological conditions for the ethanol reflux extraction were ethanol concentration was 63 %,the ratio of the material to liquid was 1 ∶ 58(g/mL),the extraction temperature was 60 ℃ and the extraction time was 120 min,under this conditions the maximum extraction yield of the total flavonoids was 11.53 %. The optimum technological conditions for the ultrasonic ethanol extraction were as follows:the ethanol concentration was 68.9 %,the ratio of the material to liquid was 1 ∶ 30(g/mL),the ultrasonic power was 73.9 W,the extraction temperature was62.2 ℃,and the extraction time was 67.7 min,under this conditions the best extraction rate of flavonoids from sweet tea was 12.23 %. Compared with the three extraction methods,the average extraction yield of ultrasonic ethanol extraction method was 12.23 % > the average extraction yield of ethanol hot reflux extraction was11.53 % > the average extraction yield of cellulase ethanol extraction was 10.89 %,the difference between the three extraction methods on the yield of total flavonoids of sweet tea reached a high(very)significant level.
In order to optimize the extraction process of total flavonoids in sweet tea,the extraction process of cellulase ethanol extraction,ethanol hot reflux extraction and ultrasonic ethanol extraction was optimized. The experiment was carried out by the combination of single factor and uniform design method. The extraction rate of total flavonoids in sweet tea was taken as the index,and the experimental data of uniform design were regressed analysis and two polynomial stepwise regression analysis. The experimental results showed that the optimum technological conditions for the extraction of cellulase and ethanol were enzyme addition was 4.3 mg(0.86 %),the pH value of the hydrolysate was 5.4,the hydrolysis temperature was 42 ℃,and the enzymolysis time was65 min,under this conditions the maximum extraction yield of the total flavonoids was 10.89 %. The optimum technological conditions for the ethanol reflux extraction were ethanol concentration was 63 %,the ratio of the material to liquid was 1 ∶ 58(g/mL),the extraction temperature was 60 ℃ and the extraction time was 120 min,under this conditions the maximum extraction yield of the total flavonoids was 11.53 %. The optimum technological conditions for the ultrasonic ethanol extraction were as follows:the ethanol concentration was 68.9 %,the ratio of the material to liquid was 1 ∶ 30(g/mL),the ultrasonic power was 73.9 W,the extraction temperature was62.2 ℃,and the extraction time was 67.7 min,under this conditions the best extraction rate of flavonoids from sweet tea was 12.23 %. Compared with the three extraction methods,the average extraction yield of ultrasonic ethanol extraction method was 12.23 % > the average extraction yield of ethanol hot reflux extraction was11.53 % > the average extraction yield of cellulase ethanol extraction was 10.89 %,the difference between the three extraction methods on the yield of total flavonoids of sweet tea reached a high(very)significant level.
引文
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[17]王帅,程建军,倪春蕾,等.乳酸菌对玉米加工特性的影响及基于均匀设计优化玉米发酵条件[J].食品工业科技,2016,37(13):183-187,191
[18]叶韬,王云,林琳,等.即食罗非鱼粒的熟制、成型及其调味的研究[J].现代食品科技,2016,32(3):252-258
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[20]张黎明,李瑞超,郝利民,等.响应面优化玛咖叶总黄酮提取工艺及其抗氧化活性研究[J].现代食品科技,2014,30(4):233-239
[21]孙海燕.樱桃核中类黄酮快速溶剂萃取工艺优化及抗氧化研究[J].食品工业,2017,38(8):106-109
[22]Lachlan J Schwarz,Basil Danylec,Yuanzhong Yang.Enrichment of(E)-resveratrol from peanut byproduct with molecularly imprinted polymers[J].Journal of Agricultural and Food Chemistry,2011,59(8):3539-3543
[23]陈丛瑾,杨国恩.高速逆流色谱法分离纯化黄酮类化合物的研究进展[J].西北药学杂志,2011,26(4):306-310
[24]盛占武,孙志高,黄学根,等.超滤法提取橙皮苷工艺研究[J].食品科学,2008,29(2):188-191
[25]郭丽琼,苏霞,蒋国林.柑橘类黄酮提取方法的研究进展[J].食品工业科技,2012,33(14):412-420
[2]鲍晨阳.甜茶中主要活性成分提取、纯化工艺的研究[D].贵阳:贵州师范大学,2016
[3]WANG SHIOW T,CHEN C T,SCIARAPPA W,et al.Fruit quality,antioxidant capacity,and flavonoid content of organically and conventionally grown blueberries[J].J Agric Food Chem,2008,56(14):5788-5794
[4]王雪飞,张华.多酚类物质生理功能的研究进展[J].食品研究与开发,2012,33(2):211-214
[5]左玉.多酚类化合物研究进展[J].粮食与油脂,2013,26(4):6-10
[6]李祝,陈蓉,李猷,等.广西甜茶中甜茶素的提取工艺研究[J].食品工业,2013(2):93-95
[7]李玉龙,杨烨,陆国权.基于均匀设计和主成分分析的甘薯薯片油炸工艺优化[J].食品科学,2017,38(4):223-230
[8]吴祥庭,董新姣,杨海龙,等.山药皂甙均匀设计法优化提取及其体外抗氧化活性研究[J].中国食品学报,2013,13(2):91-96
[9]方开泰.正交与均匀试验设计[M].北京:科学出版社,2001:35-39,83-85
[10]钟政昌,王腾飞,方江平.均匀设计法优化西藏光核桃原果浆保鲜配方[J].食品科技,2014,39(5):47-51
[11]Turkmen N,Sari F,Veliouglu Y S.Effects of extraction solvents on concentration and antioxidant activity of black and black mate tea polyphenols determined by ferrous tartrate and Folin-Ciocalteu methods[J].Food Chemistry,2006,99:835-841
[12]赫锦锦,张木升,杜红岩,等.分光光度法测定杜仲雄花中总黄酮的含量[J].河南大学学报,2011(1):11-13
[13]王静霞,黄艳菲,赵小燕,等.荞麦和商品苦荞茶中总黄酮的含量测定[J].食品工业科技,2013,34(2):58-60
[14]程雅芳,杨洋,韦银凤,等.超声波辅助提取甜茶黄酮的工艺优化[J].食品科技,2011,36(4):189-196
[15]Jianxiong Y,Chen Y,Juan Q,et al.In vitro Antioxidantproperties of Forsythia suspense Leaves flavonoids[J].Natural Products Research and Development,2007,19:97-100
[16]Pan X,Niu G,Liu H.Microwave-assisted extraction of tea polyphenols and tea caffeine from green tea leaves[J].Chemical Engineering and Processing,2003,42(2):129-133
[17]王帅,程建军,倪春蕾,等.乳酸菌对玉米加工特性的影响及基于均匀设计优化玉米发酵条件[J].食品工业科技,2016,37(13):183-187,191
[18]叶韬,王云,林琳,等.即食罗非鱼粒的熟制、成型及其调味的研究[J].现代食品科技,2016,32(3):252-258
[19]Wu J C,Cheng J,Shi X,et al.Preparation of ACE inhibitory peptides from Mytilus coruscus hydrolysate using uniform design[J].Bio Med Research International,2013,2013:1-6
[20]张黎明,李瑞超,郝利民,等.响应面优化玛咖叶总黄酮提取工艺及其抗氧化活性研究[J].现代食品科技,2014,30(4):233-239
[21]孙海燕.樱桃核中类黄酮快速溶剂萃取工艺优化及抗氧化研究[J].食品工业,2017,38(8):106-109
[22]Lachlan J Schwarz,Basil Danylec,Yuanzhong Yang.Enrichment of(E)-resveratrol from peanut byproduct with molecularly imprinted polymers[J].Journal of Agricultural and Food Chemistry,2011,59(8):3539-3543
[23]陈丛瑾,杨国恩.高速逆流色谱法分离纯化黄酮类化合物的研究进展[J].西北药学杂志,2011,26(4):306-310
[24]盛占武,孙志高,黄学根,等.超滤法提取橙皮苷工艺研究[J].食品科学,2008,29(2):188-191
[25]郭丽琼,苏霞,蒋国林.柑橘类黄酮提取方法的研究进展[J].食品工业科技,2012,33(14):412-420