不同提取方法对黄秋葵果胶含量和结构特性的影响
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摘要
本研究探讨了酸水热提、酶解、超声及酶解-超声四种提取方法对黄秋葵果胶含量及其结构特性的影响。酸水热提及酶解-超声联合法对黄秋葵果胶提取效果优于酶解和超声法;当干秋葵加入20倍pH 3 HCl水溶液,以70℃浸提1h(酸水热提法)或添加3‰果胶酶、50℃酶解90min后置于200W超声波处理10min(酶解-超声法)时,其果胶平均含量(以半乳糖醛酸质量分数计)达到43.61g/kg及32.59g/kg。四种提取方法所制果胶均为吡喃糖构型,但酸水热提及酶解法制备果胶的酯键易发生降解,其在1725cm~(-1)红外吸收峰有变弱甚至消失趋势;而超声或酶解-超声法处理则促进了果胶分子链断裂,其平均分子量由酸水热提法下533ku分别降至420～467ku、319ku。研究结果表明:采用酸水热提法(pH 3、70℃)制备黄秋葵果胶,其果胶得率高、分子量分布集中、外观呈片状且排列致密。本研究结果为高品质秋葵果胶的制备奠定基础。
The effects of four extraction methods such as hot acid-water extraction, enzymolysis, ultrasound, and enzymolysis-ultrasound treatment on the content and structural characteristics of the pectins from okra were studied, and the hot acid-water extraction and enzymolysis-ultrasound methods were found more effective. At the ratio of dried okra to the HCl aqueous solution(pH 3) of 1:20, the extraction at 70 ℃ for 1 h(the hot acid-water extraction method) or with addition of 3‰ of pectinase, and the digestion at 50 ℃ for 90 min followed by an ultrasound treatment at 200 W for 10 min(the enzymolysis-ultrasound method), led to a pectin content(as the galacturonic acid mass in okra) of 43.61 and 32.59 g/kg, respectively. All the pectins produced by the four extraction methods was in the pyranose configuration, but the ester bond in the pectins prepared via the hot acid-water extraction or the enzymolysis method tended to degrade, causing the infra-red adsorption peak at 1725 cm~(-1) to be weakened or even disappear. Whereas, the ultrasound methods or enzymolysis-ultrasound treatment promoted the breakage of the pectin molecular chain, making its average molecular weight decrease from 533 ku(by the hot acid-water method) to 420～467 ku and 319 ku. The results showed that the okra pectin prepared via the hot acid-water extraction method had a higher extraction yield and narrow molecular weight distribution with a flake-like and densely arranged appearance. The results of this research has laid the foundation for the preparation of high quality okra pectin.
The effects of four extraction methods such as hot acid-water extraction, enzymolysis, ultrasound, and enzymolysis-ultrasound treatment on the content and structural characteristics of the pectins from okra were studied, and the hot acid-water extraction and enzymolysis-ultrasound methods were found more effective. At the ratio of dried okra to the HCl aqueous solution(pH 3) of 1:20, the extraction at 70 ℃ for 1 h(the hot acid-water extraction method) or with addition of 3‰ of pectinase, and the digestion at 50 ℃ for 90 min followed by an ultrasound treatment at 200 W for 10 min(the enzymolysis-ultrasound method), led to a pectin content(as the galacturonic acid mass in okra) of 43.61 and 32.59 g/kg, respectively. All the pectins produced by the four extraction methods was in the pyranose configuration, but the ester bond in the pectins prepared via the hot acid-water extraction or the enzymolysis method tended to degrade, causing the infra-red adsorption peak at 1725 cm~(-1) to be weakened or even disappear. Whereas, the ultrasound methods or enzymolysis-ultrasound treatment promoted the breakage of the pectin molecular chain, making its average molecular weight decrease from 533 ku(by the hot acid-water method) to 420～467 ku and 319 ku. The results showed that the okra pectin prepared via the hot acid-water extraction method had a higher extraction yield and narrow molecular weight distribution with a flake-like and densely arranged appearance. The results of this research has laid the foundation for the preparation of high quality okra pectin.
引文
[1]薛志忠,刘思雨,杨雅华.黄秋葵的应用价值与开发利用研究进展[J].保鲜与加工,2013,13(2):58-60XUE Zhi-zhong,LIU Si-yu,YANG Ya-hua.Research progress on application value and development of Okra[J].Storage&Process,2013,13(2):58-60
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[3]韩菊兰,李臻,胡韬,等.黄秋葵的功能特性及综合[J].现代农业科技,2013,3:105-106HAN Ju-lan,LI Zhen,HU Tao,et al.Functional characteristics and comprehensive application of Okra[J].Modern Agricultural Technology,2013,3:105-106
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[5]周倩,何小维,罗志刚.果胶的制备及其应用[J].食品工业科技,2007,28(9):240-243ZHOU Qian,HE Xiao-wei,LUO Zhi-gang.Research on preparation and application of pectin[J].Science and Technology of Food Industry,2007,28(9):240-243
[6]Schols H A,Bakx E J,Schipper D,et al.A xylogalacturonan subunit present in the modified hairy regions of apple pectin[J].Carbohydrate Research,1995,279(1):265-279
[7]谢明勇,李精,聂少平.果胶研究与应用进展[J].中国食品学报,2013,13(8):1-14XIE Ming-yong,LI Jing,NIE Shao-ping.A Review about the research and applications of pectin[J].Journal of Chinese Institute of Food Science and Technology,2013,13(8):1-14
[8]Munarin F,Tanzi M C,Petrini P.Advances in biomedical applications of pectin gels[J].International Journal of Biological Macromolecules,2012,51(4):681-689
[9]GUO X,HAN D,XI H,et al.Extraction of pectin from navel orange peel assisted by ultra-high pressure,microwave or traditional heating:A comparison[J].Carbohydrate Polymers,2012,88(2):441-448
[10]王慧,罗翀,王征.酶法提取植物果胶研究进展[J].生物技术世界,2013,5:65-65WANG Hui,LUO Chong,WANG Zheng.Advances in enzymatic extraction of plant pectin[J].Biotechnology World,2013,5:65-65
[11]刘海霞.黄秋葵花果胶类多糖的提取工艺及其性质的研究[D].杭州:浙江大学,2014LIU Hai-xia.Study on extraction process and properties of pectin polysaccharides from Okra[D].Hangzhou:Zhejiang University,2014
[12]黄剑波,孙哲浩,张英慧,等.黄秋葵果胶提取工艺的初步研究[J].现代食品科技,2007,23(2):57-59HUANG Jian-bo,SUN Ze-hao,ZHANG Ying-hui,et al.Study on extraction of pectin from Okra[J].Modern Food Science and Technology,2007,23(2):57-59
[13]周小敏,许鑫,郭天立,等.不同提取方法对黄秋葵果胶理化性质影响[J].食品工业,2018,39(2):54-57ZHOU Xiao-min,XU Xin,GUO Tian-li,et al.Effects of different extraction methods on physical and chemical properties of okra pectin[J].The Food Industry,2018,39(2):54-57
[14]吴建花,尹红,黄诚.黄秋葵中果胶提取工艺研究[J].现代农业科技,2017,11:246-248WU Jian-hua,YIN Hong,HUANG Cheng.Research on extraction technology of pectin from Abelmoschus esculentus(Linn.)Moench[J].Modern Agricultural Science and Technology,2017,11:246-248
[15]李加兴,覃敏杰,吴越,等.响应面法优化黄秋葵果胶微波辅助提取工艺[J].食品科学,2013,34(14):12-16LI Jia-xing,QIN Min-jie,WU Yue,et al.Optimization of microwave-assisted extraction conditions for pectin from Okra by response surface methodology[J].Food Science,2013,34(14):12-16
[16]黄梓琪,吴湛霞,林宏图,等.微波辅助草酸铵提取黄秋葵果胶的工艺研究[J].广州化工,2015,17:77-79HUANG Zi-qi,WU Zhan-xia,LIN Hong-tu,et al.Study on the process of extracting pectin from Okra with microwave-assisted ammonium oxalate[J].Guangzhou Chemical Industry and Technology,2015,17:77-79
[17]王炜强,李本刚,罗振扬,等.黄秋葵多糖提取及其絮凝性能[J].食品工业科技,2017,21:76-79WANG Wei-qiang,LI Ben-gang,LUO Zhen-yang,et al.Extraction and flocculation properties of okra polysaccharide[J].Science and Technology of Food Industry,2017,21:76-79
[18]于梅,单凌越,井瑞洁,等.黄秋葵超微粉多糖提取工艺的优化及其抗氧化活性测定[J].食品工业科技,2018,7:175-180YU Mei,DAN Ling-yue,JING Rui-jie,et al.Optimization of extraction technology and determination of antioxidant activity of polysaccharides from superfine powder of okra[J].Science and Technology of Food Industry,2018,7:175-180
[19]陈剑兵,尹颖,陆胜民,等.亚临界水处理制备低分子柑橘果胶及其性质研究[J].现代食品科技,2014,30(6):186-190CHEN Jian-bing,YIN Ying,LU Sheng-min,et al.Subcritical water preparation and properties of low molecular citrus pectin[J].Modern Food Science and Technology,2014,30(6):186-190
[20]梁瑞红,王玲华,帅希祥,等.动态高压微射流处理对低酯果胶物化性质及其结构的影响[J].现代食品科技,2015,31(1):115-119LIANG Rui-hong,WANG Ling-hua,SHUAI Xi-xiang,et al.Effects of dynamic high-pressure microfluidization on the physicochemical properties and structure of low-methoxyl Pectin[J].Modern Food Science and Technology,2015,31(1):115-119
[21]刘战朋,郭晓明,皮芳,等.果胶提取工艺对甜菜粕物化性质的修饰作用研究[J].现代食品科技,2018,34(1):68-74LIU Zhan-peng,GUO Xiao-ming,PI Fang,et al.Modification of pectin extraction conditions on physiochemical properties of sugar beet pulp[J].Modern Food Science and Technology,2018,34(1):68-74
[22]Fraeye I,Ade R,Duvetter T,et al.Influence of pectin properties and processing conditions on thermal pectin degradation[J].Food Chemistry,2007,105(2):555-563
[23]郭兴峰,赵文婷,廖小军,等.酸性条件下热处理对果胶流变和结构特性的影响[J].食品科学,2018,39(12):40-46GUO Xing-feng,ZHAO Wen-ting,LIAO Xiao-jun,et al.Effect of heat treatment under acidic condition on the rheological and structural characteristics of pectin[J].Food Science,2018,39(12):40-46
[24]De R A,Sila D N,Duvetter T,et al.Effect of high pressure/high temperature processing on cell wall pectic substances in relation to firmness of carrot tissue[J].Food Chemistry,2008,107(3):1225-1235
[25]CHEN J,LIANG R H,LIU W,et al.Degradation of high-methoxyl pectin by dynamic high pressure microfluidization and its mechanism[J].Food Hydrocolloids,2012,28(1):121-129
[26]NY/T 2016-2011,水果及其制品中果胶含量的测定,分光光度法[S]NY/T 2016-2011,Fruit and its Products-determination of Pectin Content,Spectrophotometry[S]
[27]陈忆.黄秋葵果胶和超微粉的制备及性质研究[D].合肥:合肥工业大学,2015CHEN Yi.Preparation and properties of Okra pectin and ultrafine powder[D].Hefei:Hefei University of Technology,2015
[28]ZHANG L,YE X,DING T,et al.Ultrasound effects on the degradation kinetics,structure and rheological properties of apple pectin[J].Ultrasonics Sonochemistry,2013,20(1):222-231
[29]JIANG C M,LAIY J,LEE B H,et al.Changes in physico-chemical properties of pectin from jelly fig(Ficus awkeotsang Makino)seeds during extraction and gelling[J].Food Research International,2002,35(1):31-35
[30]Ebringerova A,Hromadkova Z.An overview on the application of ultrasound in extraction,separation and purification of plant polysaccharides[J].Central European Journal of Chemistry,2010,8(2):243-257
[31]张丽芬.果胶多糖超声波定向降解途径及机理研究[D].杭州:浙江大学,2013ZHANG Li-fen.Study on the pathway and mechanism of ultrasonic directed degradation of pectin polysaccharide[D].Hangzhou:Zhejiang University,2013
[32]Manrique G D,Lajolo F M.FT-IR spectroscopy as a tool for measuring degree of methylesterification in pectins isolated from ripening papaya fruit[J].Postharvest Biology and Technology,2002,25(1):99-107
[33]孙元琳,崔武惟,顾小红,等.傅里叶变换红外光谱法测定当归果胶多糖的酯化度[J].光谱学与光谱分析,2009,29(3):682-685SUN Yuan-lin,CUI Wu-wei,GU Xiao-hong,et al.Determination of degree of esterification in pectic polysaccharides from Angelica sinensis Diels by fourier transform infrared spectroscopy[J].Spectroscopy and Spectral Analysis,2009,29(3):682-685
[34]Thakur B R,Singh R K,Handa A K.Chemistry and uses of pectin:a review[J].Critical Reviews in Food Science and Nutrition,1997,37(1):47-73
[2]高玲,刘迪发,徐丽.黄秋葵研究进展与前景[J].热带农业科学,2014,34(11):22-29GAO Ling,LIU Di-fa,XU Li.Research progress and prospects of Okra[J].Chinese Journal of Tropical Agriculture,2014,34(11):22-29
[3]韩菊兰,李臻,胡韬,等.黄秋葵的功能特性及综合[J].现代农业科技,2013,3:105-106HAN Ju-lan,LI Zhen,HU Tao,et al.Functional characteristics and comprehensive application of Okra[J].Modern Agricultural Technology,2013,3:105-106
[4]Caffall K H,Mohnen D.The structure,function,and biosynthesis of plant cell wall pectic polysaccharides[J].Carbohydrate Research,2009,344(14):1879-1900
[5]周倩,何小维,罗志刚.果胶的制备及其应用[J].食品工业科技,2007,28(9):240-243ZHOU Qian,HE Xiao-wei,LUO Zhi-gang.Research on preparation and application of pectin[J].Science and Technology of Food Industry,2007,28(9):240-243
[6]Schols H A,Bakx E J,Schipper D,et al.A xylogalacturonan subunit present in the modified hairy regions of apple pectin[J].Carbohydrate Research,1995,279(1):265-279
[7]谢明勇,李精,聂少平.果胶研究与应用进展[J].中国食品学报,2013,13(8):1-14XIE Ming-yong,LI Jing,NIE Shao-ping.A Review about the research and applications of pectin[J].Journal of Chinese Institute of Food Science and Technology,2013,13(8):1-14
[8]Munarin F,Tanzi M C,Petrini P.Advances in biomedical applications of pectin gels[J].International Journal of Biological Macromolecules,2012,51(4):681-689
[9]GUO X,HAN D,XI H,et al.Extraction of pectin from navel orange peel assisted by ultra-high pressure,microwave or traditional heating:A comparison[J].Carbohydrate Polymers,2012,88(2):441-448
[10]王慧,罗翀,王征.酶法提取植物果胶研究进展[J].生物技术世界,2013,5:65-65WANG Hui,LUO Chong,WANG Zheng.Advances in enzymatic extraction of plant pectin[J].Biotechnology World,2013,5:65-65
[11]刘海霞.黄秋葵花果胶类多糖的提取工艺及其性质的研究[D].杭州:浙江大学,2014LIU Hai-xia.Study on extraction process and properties of pectin polysaccharides from Okra[D].Hangzhou:Zhejiang University,2014
[12]黄剑波,孙哲浩,张英慧,等.黄秋葵果胶提取工艺的初步研究[J].现代食品科技,2007,23(2):57-59HUANG Jian-bo,SUN Ze-hao,ZHANG Ying-hui,et al.Study on extraction of pectin from Okra[J].Modern Food Science and Technology,2007,23(2):57-59
[13]周小敏,许鑫,郭天立,等.不同提取方法对黄秋葵果胶理化性质影响[J].食品工业,2018,39(2):54-57ZHOU Xiao-min,XU Xin,GUO Tian-li,et al.Effects of different extraction methods on physical and chemical properties of okra pectin[J].The Food Industry,2018,39(2):54-57
[14]吴建花,尹红,黄诚.黄秋葵中果胶提取工艺研究[J].现代农业科技,2017,11:246-248WU Jian-hua,YIN Hong,HUANG Cheng.Research on extraction technology of pectin from Abelmoschus esculentus(Linn.)Moench[J].Modern Agricultural Science and Technology,2017,11:246-248
[15]李加兴,覃敏杰,吴越,等.响应面法优化黄秋葵果胶微波辅助提取工艺[J].食品科学,2013,34(14):12-16LI Jia-xing,QIN Min-jie,WU Yue,et al.Optimization of microwave-assisted extraction conditions for pectin from Okra by response surface methodology[J].Food Science,2013,34(14):12-16
[16]黄梓琪,吴湛霞,林宏图,等.微波辅助草酸铵提取黄秋葵果胶的工艺研究[J].广州化工,2015,17:77-79HUANG Zi-qi,WU Zhan-xia,LIN Hong-tu,et al.Study on the process of extracting pectin from Okra with microwave-assisted ammonium oxalate[J].Guangzhou Chemical Industry and Technology,2015,17:77-79
[17]王炜强,李本刚,罗振扬,等.黄秋葵多糖提取及其絮凝性能[J].食品工业科技,2017,21:76-79WANG Wei-qiang,LI Ben-gang,LUO Zhen-yang,et al.Extraction and flocculation properties of okra polysaccharide[J].Science and Technology of Food Industry,2017,21:76-79
[18]于梅,单凌越,井瑞洁,等.黄秋葵超微粉多糖提取工艺的优化及其抗氧化活性测定[J].食品工业科技,2018,7:175-180YU Mei,DAN Ling-yue,JING Rui-jie,et al.Optimization of extraction technology and determination of antioxidant activity of polysaccharides from superfine powder of okra[J].Science and Technology of Food Industry,2018,7:175-180
[19]陈剑兵,尹颖,陆胜民,等.亚临界水处理制备低分子柑橘果胶及其性质研究[J].现代食品科技,2014,30(6):186-190CHEN Jian-bing,YIN Ying,LU Sheng-min,et al.Subcritical water preparation and properties of low molecular citrus pectin[J].Modern Food Science and Technology,2014,30(6):186-190
[20]梁瑞红,王玲华,帅希祥,等.动态高压微射流处理对低酯果胶物化性质及其结构的影响[J].现代食品科技,2015,31(1):115-119LIANG Rui-hong,WANG Ling-hua,SHUAI Xi-xiang,et al.Effects of dynamic high-pressure microfluidization on the physicochemical properties and structure of low-methoxyl Pectin[J].Modern Food Science and Technology,2015,31(1):115-119
[21]刘战朋,郭晓明,皮芳,等.果胶提取工艺对甜菜粕物化性质的修饰作用研究[J].现代食品科技,2018,34(1):68-74LIU Zhan-peng,GUO Xiao-ming,PI Fang,et al.Modification of pectin extraction conditions on physiochemical properties of sugar beet pulp[J].Modern Food Science and Technology,2018,34(1):68-74
[22]Fraeye I,Ade R,Duvetter T,et al.Influence of pectin properties and processing conditions on thermal pectin degradation[J].Food Chemistry,2007,105(2):555-563
[23]郭兴峰,赵文婷,廖小军,等.酸性条件下热处理对果胶流变和结构特性的影响[J].食品科学,2018,39(12):40-46GUO Xing-feng,ZHAO Wen-ting,LIAO Xiao-jun,et al.Effect of heat treatment under acidic condition on the rheological and structural characteristics of pectin[J].Food Science,2018,39(12):40-46
[24]De R A,Sila D N,Duvetter T,et al.Effect of high pressure/high temperature processing on cell wall pectic substances in relation to firmness of carrot tissue[J].Food Chemistry,2008,107(3):1225-1235
[25]CHEN J,LIANG R H,LIU W,et al.Degradation of high-methoxyl pectin by dynamic high pressure microfluidization and its mechanism[J].Food Hydrocolloids,2012,28(1):121-129
[26]NY/T 2016-2011,水果及其制品中果胶含量的测定,分光光度法[S]NY/T 2016-2011,Fruit and its Products-determination of Pectin Content,Spectrophotometry[S]
[27]陈忆.黄秋葵果胶和超微粉的制备及性质研究[D].合肥:合肥工业大学,2015CHEN Yi.Preparation and properties of Okra pectin and ultrafine powder[D].Hefei:Hefei University of Technology,2015
[28]ZHANG L,YE X,DING T,et al.Ultrasound effects on the degradation kinetics,structure and rheological properties of apple pectin[J].Ultrasonics Sonochemistry,2013,20(1):222-231
[29]JIANG C M,LAIY J,LEE B H,et al.Changes in physico-chemical properties of pectin from jelly fig(Ficus awkeotsang Makino)seeds during extraction and gelling[J].Food Research International,2002,35(1):31-35
[30]Ebringerova A,Hromadkova Z.An overview on the application of ultrasound in extraction,separation and purification of plant polysaccharides[J].Central European Journal of Chemistry,2010,8(2):243-257
[31]张丽芬.果胶多糖超声波定向降解途径及机理研究[D].杭州:浙江大学,2013ZHANG Li-fen.Study on the pathway and mechanism of ultrasonic directed degradation of pectin polysaccharide[D].Hangzhou:Zhejiang University,2013
[32]Manrique G D,Lajolo F M.FT-IR spectroscopy as a tool for measuring degree of methylesterification in pectins isolated from ripening papaya fruit[J].Postharvest Biology and Technology,2002,25(1):99-107
[33]孙元琳,崔武惟,顾小红,等.傅里叶变换红外光谱法测定当归果胶多糖的酯化度[J].光谱学与光谱分析,2009,29(3):682-685SUN Yuan-lin,CUI Wu-wei,GU Xiao-hong,et al.Determination of degree of esterification in pectic polysaccharides from Angelica sinensis Diels by fourier transform infrared spectroscopy[J].Spectroscopy and Spectral Analysis,2009,29(3):682-685
[34]Thakur B R,Singh R K,Handa A K.Chemistry and uses of pectin:a review[J].Critical Reviews in Food Science and Nutrition,1997,37(1):47-73