响应面法优化超声波辅助提取广西大果山楂叶黄酮工艺
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摘要
【目的】优化超声波辅助提取广西大果山楂叶黄酮的工艺条件,为广西大果山楂叶资源的开发利用提供技术参考。【方法】以广西大果山楂叶为原料,以超纯水为提取剂,通过单因素及响应面试验对超声波辅助提取山楂叶黄酮工艺进行优化,探讨超声波功率、提取温度、提取时间和料液比4个因素对黄酮提取率的影响。【结果】通过响应面试验建立二次多项回归方程:Y=52.91+1.41A+1.08B+1.63C+0.51AB+0.89AC+0.052BC-4.53A2-0.97B2-1.36C2(Y为黄酮提取率,A为提取温度,B为提取时间,C为料液比)。超声波辅助提取广西大果山楂叶黄酮的最佳工艺条件为:超声波功率140 W、提取温度59℃、提取时间120 min、料液比1∶56(g/m L),在此条件下黄酮提取率为54.18 mg/g,与预测值53.86 mg/g的误差小。3个因素对广西大果山楂叶黄酮提取率影响主次排序为料液比>提取温度>提取时间,提取温度与料液比的交互作用对山楂叶黄酮提取率有显著影响(P<0.05)。【结论】响应面优化得到的超声波辅助水提广西大果山楂叶黄酮工艺具有提取率高、精度高、工艺稳定的优点,可在生产中推广应用。
【Objective】The technology condition of ultrasonic-assisted extraction of flavonoids from Guangxi big fruit hawthorn leaves was optimized in order to provide technical reference for the resource utilization of Guangxi big fruit hawthorn leaves.【Method】The ultrasonic-assisted extraction of flavonoids from hawthorn leaves was optimized by using single factor and response surface test,taking the Guangxi big fruit hawthorn leaves as the raw material,and ultra-pure water as the extractant. The effects of four factors including ultrasonic power,extraction temperature,extraction time and solid liquid ratio on extraction rate of flavonoids were studied.【Result】According to response surface test,the quadratic regression model equation was established:Y=52.91 +1.41 A +1.08 B +1.63 C +0.51 AB +0.89 AC +0.052 BC-4.53 A2-0.97 B2-1.36 C2(Y referred to the extraction rate of flavonoids;A referred to extraction temperature;B referred to extraction time;and C referred to solid liquid ratio). The optimum technology conditions for ultrasonic-assisted extraction of flavonoids from big fruit hawthorn leaves were as follows:the ultrasonic power was 140 W;the extraction temperature 59 ℃;extraction time 120 min and solid liquid ratio 1∶56(g/m L). Under such conditions,the extraction rate of flavonoid was 54.18 mg/g and the error was small compared with the predictive value(53.86 mg/g). According to importance order,the influence of the three factors on the extraction rate of flavonoids from Guangxi big fruit hawthorn leaves was solid liquid ratio>extraction temperature>extraction time. And the interaction between extraction temperature and solid-liquid ratio had significant influence on the extraction rate of flavonoids from hawthorn leaves(P<0.05).【Conclusion】The ultrasonic-assisted water extraction optimized by response surface has following advantages:high extraction rate,high precision and stable technology,so it can be used for the promotion and application in production.
【Objective】The technology condition of ultrasonic-assisted extraction of flavonoids from Guangxi big fruit hawthorn leaves was optimized in order to provide technical reference for the resource utilization of Guangxi big fruit hawthorn leaves.【Method】The ultrasonic-assisted extraction of flavonoids from hawthorn leaves was optimized by using single factor and response surface test,taking the Guangxi big fruit hawthorn leaves as the raw material,and ultra-pure water as the extractant. The effects of four factors including ultrasonic power,extraction temperature,extraction time and solid liquid ratio on extraction rate of flavonoids were studied.【Result】According to response surface test,the quadratic regression model equation was established:Y=52.91 +1.41 A +1.08 B +1.63 C +0.51 AB +0.89 AC +0.052 BC-4.53 A2-0.97 B2-1.36 C2(Y referred to the extraction rate of flavonoids;A referred to extraction temperature;B referred to extraction time;and C referred to solid liquid ratio). The optimum technology conditions for ultrasonic-assisted extraction of flavonoids from big fruit hawthorn leaves were as follows:the ultrasonic power was 140 W;the extraction temperature 59 ℃;extraction time 120 min and solid liquid ratio 1∶56(g/m L). Under such conditions,the extraction rate of flavonoid was 54.18 mg/g and the error was small compared with the predictive value(53.86 mg/g). According to importance order,the influence of the three factors on the extraction rate of flavonoids from Guangxi big fruit hawthorn leaves was solid liquid ratio>extraction temperature>extraction time. And the interaction between extraction temperature and solid-liquid ratio had significant influence on the extraction rate of flavonoids from hawthorn leaves(P<0.05).【Conclusion】The ultrasonic-assisted water extraction optimized by response surface has following advantages:high extraction rate,high precision and stable technology,so it can be used for the promotion and application in production.
引文
曹剑锋,芦静波,滕树学,任朝辉,陈慧琴.2016.密蒙花总黄酮的抗氧化及免疫调节作用[J].河南农业科学,45(9):130-134.[Cao J F,Lu J B,Teng S X,Ren C H,Chen HQ.2016.Immune regulation function and antioxidant capacities of total flavonoids from Buddleja officinalis Maxim DC.[J].Journal of Henan Agricultural Sciences,45(9):130-134.]
曹乐民,周志强,崔俊林,石明生.2014.山楂叶中总黄酮的浸提工艺研究[J].中国酿造,33(2):75-77.[Cao L M,Zhou Z Q,Cui J L,Shi M S.2014.Extraction technology of flavonoids from hawthorn leaves[J].China Brewing,33(2):75-77.]
陈兵兵,梁昌祥,吴桂容.2017.大果山楂黄酮提取的方法研究[J].现代养生,(6):46-47.[Chen B B,Liang C X,Wu G R.2017.Study on the extraction of flavonoids from hawthorn fruit[J].Health Care Today,(6):46-47.]
房磊.2016.超声波辅助提取银杏叶黄酮及体外抗运动氧化作用研究[J].食品研究与开发,37(17):153-157.[Fang L.2016.Study on the ultrasonic assisted extraction of flavonoids from Ginkgo biloba and its anti-oxidation effect in vitro[J].Food Research and Development,37(17):153-157.]
郭菁菁,杨秀芬.2008.黄酮类化合物对动物实验性肝损伤保护作用的研究进展[J].中国药理学通报,24(1):5-10.[Guo J J,Yang X F.2008.Research progress of the protective effect of flavonoids on experimental liver injury in animals[J].Chinese Pharmacological Bulletin,24(1):5-10.]
郭梅,任效东,王娜,李拖平.2012.微波辅助提取山楂黄酮类化合物的工艺[J].食品研究与开发,33(3):51-53.[Guo M,Ren X D,Wang N,Li T P.2012.Study on microwave assisted extraction of total flavonoids from hawthorn fruits[J].Food Research and Development,33(3):51-53.]
韩秋菊.2011.微波辅助法提取山楂黄酮类化合物的工艺条件研究[J].安徽农业科学,39(14):8612-8614.[Han QJ.2011.Study of flavonoids extraction from hawkthorn by microwave extraction method[J].Journal of Anhui Agricultural Sciences,39(14):8612-8614.]
侯学敏,李林霞,张直峰,闫桂琴.2013.响应面法优化薄荷叶总黄酮提取工艺及抗氧化活性[J].食品科学,34(6):124-128.[Hou X M,Li L X,Zhang Z F,Yan G Q.2013.Total flavonoids from Mentha haplocalyx Briq.leaves:Optimization of extraction process by response surface methodology and antioxidant activity[J].Food Science,34(6):124-128.]
黄欣欣,叶志青,郭兵兵,文良娟.2015.响应面法优化回流提取大果山楂总黄酮工艺[J].南方农业学报,46(6):1089-1095.[Huang X X,Ye Z Q,Guo B B,Wen L J.2015.Reflux extraction process optimization of total flavonoids from Malus domeri(Bois)Chev.fruits by response surface methodology[J].Journal of Southern Agriculture,46(6):1089-1095.]
姜晓娇,王承明.2010.响应面优化脱酚棉籽粕制备棉籽多肽研究[J].中国油脂,35(6):22-26.[Jiang X J,Wang CM.2010.Preparation of peptides from degossypoled cottonseed meal by response surface methodology[J].Chinese Oils and Fats,35(6):22-26.]
李春荣,孟铁宏,罗亚男,姜艳萍,任竹君,杨勤.2016.超声提取乌纠黄酮的工艺优化[J].贵州农业科学,44(9):132-139.[Li C R,Meng T H,Luo Y N,Jiang Y P,Ren Z J,Yang Q.2016.Optimization of ultrasonic-assisted extraction technology of flavonoids from Wet jiub[J].Guizhou Agricultural Sciences,44(9):132-139.]
李宁豫,韩秋菊,曹月坤.2013.超声辅助提取山楂黄酮的研究[J].陕西农业科学,59(3):91-93.[Li N Y,Han Q J,Cao Y K.2013.Ultrasound-assisted extraction of hawthorn flavonoids[J].Shaanxi Journal of Agricultural Sciences,59(3):91-93.]
刘伟,欧阳艳,何晓燕,王运莲,刘晓,周双傲,王永平.2016.准噶尔山楂叶总黄酮提取、测定及抗氧化活性研究[J].伊犁师范学院学报(自然科学版),10(2):59-64.[Liu W,Ouyang Y,He X Y,Wang Y L,Liu X,Zhou S A,Wang Y P.2016.Extraction,determination and antioxidant activity of total flavonoids from Crataegus songorica leaves[J].Journal of Yili Normal University(Natural Science Edition),10(2):59-64.]
施红林,黄琦,褚沈佳,库娜娜,俞小燕,王媛媛.2014.响应面分析法优化山楂叶中黄酮的提取工艺[J].浙江科技学院学报,26(3):165-171.[Shi H L,Huang Q,Chu S J,Ku N N,Yu X Y,Wang Y Y.2014.Optimization of extraction technology of flavonoids from howthorn leaves by response surface method[J].Journal of Zhejiang University of Science and Technology,26(3):165-171.]
苏曼曼,于晓风,曲绍春,徐华丽,睢大筼.2007.分蘖葱头总黄酮对实验性高脂血症大鼠血脂代谢的影响[J].中国药理学通报,23(12):1593-1597.[Su M M,Yu X F,Qu SC,Xu H L,Sui D Y.2007.Effects of TFAD on the bloodliquid metabolism in experimental hyperlipoproteinemia rats[J].Chinese Pharmacological Bulletin,23(12):1593-1597.]
夏成凯,李静,汪电雷.2014.山楂叶总黄酮制备工艺参数的研究[J].长江大学学报(自科版),11(3):79-81.[Xia CK,Li J,Wang D L.2014.A research on optimal screening of technical conditions in preparation technology of total flavonoids in hawthorn leaves[J].Journal of Yangtze University(Natural Science Edition),11(3):79-81.]
袁冬梅,李一婧.2007.山楂叶中黄酮含量的高效液相色谱法测定[J].中国酿造,26(12):66-68.[Yuan D M,Li Y J.2007.Determination of flavone content in hawthom leave by HPLC[J].China Brewing,26(12):66-68.]
张昊,邵青,贺晓龙,王延峰.2016.响应面法优化山丹鳞茎总黄酮提取工艺的研究[J].河南农业科学,45(3):152-156.[Zhang H,Shao Q,He X L,Wang Y F.2016.Optimization of extraction process of total flavonoids from Lilium pumilum bulb using response surface methodology[J].Journal of Henan Agricultural Sciences,45(3):152-156.]
赵跃刚,王隶书,范艳君,刘永宏.2011.酢浆草药材中总黄酮的含量测定[J].时珍国医国药,22(1):81-82.[Zhao YG,Wang L S,Fan Y J,Liu Y H.2011.Comparison on the contents of the total flavonoid in herba Oxalidis corniculatae[J].Lishizhen Medicine and Materia Medica Research,22(1):81-82.]
赵强,余四九,王廷璞,袁毅君.2012.响应面法优化秃疮花中生物碱提取工艺及抑菌活性研究[J].草业学报,21(4):206-214.[Zhao Q,Yu S J,Wang T P,Yuan Y J.2012.Optimization of the extracting process for alkaloids from Dicranostigma leptopodum by response surface analysis and study on its antibacterial activity in vitro[J].Acta Prataculturae Sinica,21(4):206-214.]
周海旭,高晗,曲良苗,李忠海.2011.响应面法优化山楂叶中黄酮提取工艺[J].河南农业大学学报,45(6):712-715.[Zhou H G,Gao H,Qu L M,Li Z H.2011.Optimization of flavonoids extraction from hawthorn leaves by response surface methodology[J].Journal of Henan Agricultural University,45(6):712-715.]
曹乐民,周志强,崔俊林,石明生.2014.山楂叶中总黄酮的浸提工艺研究[J].中国酿造,33(2):75-77.[Cao L M,Zhou Z Q,Cui J L,Shi M S.2014.Extraction technology of flavonoids from hawthorn leaves[J].China Brewing,33(2):75-77.]
陈兵兵,梁昌祥,吴桂容.2017.大果山楂黄酮提取的方法研究[J].现代养生,(6):46-47.[Chen B B,Liang C X,Wu G R.2017.Study on the extraction of flavonoids from hawthorn fruit[J].Health Care Today,(6):46-47.]
房磊.2016.超声波辅助提取银杏叶黄酮及体外抗运动氧化作用研究[J].食品研究与开发,37(17):153-157.[Fang L.2016.Study on the ultrasonic assisted extraction of flavonoids from Ginkgo biloba and its anti-oxidation effect in vitro[J].Food Research and Development,37(17):153-157.]
郭菁菁,杨秀芬.2008.黄酮类化合物对动物实验性肝损伤保护作用的研究进展[J].中国药理学通报,24(1):5-10.[Guo J J,Yang X F.2008.Research progress of the protective effect of flavonoids on experimental liver injury in animals[J].Chinese Pharmacological Bulletin,24(1):5-10.]
郭梅,任效东,王娜,李拖平.2012.微波辅助提取山楂黄酮类化合物的工艺[J].食品研究与开发,33(3):51-53.[Guo M,Ren X D,Wang N,Li T P.2012.Study on microwave assisted extraction of total flavonoids from hawthorn fruits[J].Food Research and Development,33(3):51-53.]
韩秋菊.2011.微波辅助法提取山楂黄酮类化合物的工艺条件研究[J].安徽农业科学,39(14):8612-8614.[Han QJ.2011.Study of flavonoids extraction from hawkthorn by microwave extraction method[J].Journal of Anhui Agricultural Sciences,39(14):8612-8614.]
侯学敏,李林霞,张直峰,闫桂琴.2013.响应面法优化薄荷叶总黄酮提取工艺及抗氧化活性[J].食品科学,34(6):124-128.[Hou X M,Li L X,Zhang Z F,Yan G Q.2013.Total flavonoids from Mentha haplocalyx Briq.leaves:Optimization of extraction process by response surface methodology and antioxidant activity[J].Food Science,34(6):124-128.]
黄欣欣,叶志青,郭兵兵,文良娟.2015.响应面法优化回流提取大果山楂总黄酮工艺[J].南方农业学报,46(6):1089-1095.[Huang X X,Ye Z Q,Guo B B,Wen L J.2015.Reflux extraction process optimization of total flavonoids from Malus domeri(Bois)Chev.fruits by response surface methodology[J].Journal of Southern Agriculture,46(6):1089-1095.]
姜晓娇,王承明.2010.响应面优化脱酚棉籽粕制备棉籽多肽研究[J].中国油脂,35(6):22-26.[Jiang X J,Wang CM.2010.Preparation of peptides from degossypoled cottonseed meal by response surface methodology[J].Chinese Oils and Fats,35(6):22-26.]
李春荣,孟铁宏,罗亚男,姜艳萍,任竹君,杨勤.2016.超声提取乌纠黄酮的工艺优化[J].贵州农业科学,44(9):132-139.[Li C R,Meng T H,Luo Y N,Jiang Y P,Ren Z J,Yang Q.2016.Optimization of ultrasonic-assisted extraction technology of flavonoids from Wet jiub[J].Guizhou Agricultural Sciences,44(9):132-139.]
李宁豫,韩秋菊,曹月坤.2013.超声辅助提取山楂黄酮的研究[J].陕西农业科学,59(3):91-93.[Li N Y,Han Q J,Cao Y K.2013.Ultrasound-assisted extraction of hawthorn flavonoids[J].Shaanxi Journal of Agricultural Sciences,59(3):91-93.]
刘伟,欧阳艳,何晓燕,王运莲,刘晓,周双傲,王永平.2016.准噶尔山楂叶总黄酮提取、测定及抗氧化活性研究[J].伊犁师范学院学报(自然科学版),10(2):59-64.[Liu W,Ouyang Y,He X Y,Wang Y L,Liu X,Zhou S A,Wang Y P.2016.Extraction,determination and antioxidant activity of total flavonoids from Crataegus songorica leaves[J].Journal of Yili Normal University(Natural Science Edition),10(2):59-64.]
施红林,黄琦,褚沈佳,库娜娜,俞小燕,王媛媛.2014.响应面分析法优化山楂叶中黄酮的提取工艺[J].浙江科技学院学报,26(3):165-171.[Shi H L,Huang Q,Chu S J,Ku N N,Yu X Y,Wang Y Y.2014.Optimization of extraction technology of flavonoids from howthorn leaves by response surface method[J].Journal of Zhejiang University of Science and Technology,26(3):165-171.]
苏曼曼,于晓风,曲绍春,徐华丽,睢大筼.2007.分蘖葱头总黄酮对实验性高脂血症大鼠血脂代谢的影响[J].中国药理学通报,23(12):1593-1597.[Su M M,Yu X F,Qu SC,Xu H L,Sui D Y.2007.Effects of TFAD on the bloodliquid metabolism in experimental hyperlipoproteinemia rats[J].Chinese Pharmacological Bulletin,23(12):1593-1597.]
夏成凯,李静,汪电雷.2014.山楂叶总黄酮制备工艺参数的研究[J].长江大学学报(自科版),11(3):79-81.[Xia CK,Li J,Wang D L.2014.A research on optimal screening of technical conditions in preparation technology of total flavonoids in hawthorn leaves[J].Journal of Yangtze University(Natural Science Edition),11(3):79-81.]
袁冬梅,李一婧.2007.山楂叶中黄酮含量的高效液相色谱法测定[J].中国酿造,26(12):66-68.[Yuan D M,Li Y J.2007.Determination of flavone content in hawthom leave by HPLC[J].China Brewing,26(12):66-68.]
张昊,邵青,贺晓龙,王延峰.2016.响应面法优化山丹鳞茎总黄酮提取工艺的研究[J].河南农业科学,45(3):152-156.[Zhang H,Shao Q,He X L,Wang Y F.2016.Optimization of extraction process of total flavonoids from Lilium pumilum bulb using response surface methodology[J].Journal of Henan Agricultural Sciences,45(3):152-156.]
赵跃刚,王隶书,范艳君,刘永宏.2011.酢浆草药材中总黄酮的含量测定[J].时珍国医国药,22(1):81-82.[Zhao YG,Wang L S,Fan Y J,Liu Y H.2011.Comparison on the contents of the total flavonoid in herba Oxalidis corniculatae[J].Lishizhen Medicine and Materia Medica Research,22(1):81-82.]
赵强,余四九,王廷璞,袁毅君.2012.响应面法优化秃疮花中生物碱提取工艺及抑菌活性研究[J].草业学报,21(4):206-214.[Zhao Q,Yu S J,Wang T P,Yuan Y J.2012.Optimization of the extracting process for alkaloids from Dicranostigma leptopodum by response surface analysis and study on its antibacterial activity in vitro[J].Acta Prataculturae Sinica,21(4):206-214.]
周海旭,高晗,曲良苗,李忠海.2011.响应面法优化山楂叶中黄酮提取工艺[J].河南农业大学学报,45(6):712-715.[Zhou H G,Gao H,Qu L M,Li Z H.2011.Optimization of flavonoids extraction from hawthorn leaves by response surface methodology[J].Journal of Henan Agricultural University,45(6):712-715.]