NKA-9大孔树脂对绿豆皮黄酮的纯化研究
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摘要
以绿豆皮黄酮为对象,通过静态吸附研究其在大孔树脂NKA-9上的吸附特性。吸附动力学结果表明,准二级动力学模型(R2>0.99)能够较好地描述绿豆皮黄酮在NKA-9树脂上的吸附过程,其吸附等温线符合Langmuir等温吸附方程(R2>0.99)。通过动态吸附和解吸试验,得到绿豆皮黄酮的最佳工艺参数为:2 BV质量浓度为0.4 mg/mL的绿豆皮黄酮提取液(pH 3),上样流速2 BV/h,用2.3 BV 70%的乙醇溶液(pH 5)为洗脱剂,以2BV/h进行洗脱,在此条件下,绿豆皮黄酮的纯度由28.26%上升到75.74%,总黄酮的回收率由24.56%上升到64.91%。高效液相色谱分析表明,牡荆素和异牡荆素是绿豆皮黄酮提取液的主要成分,经NKA-9树脂纯化后,纯度显著提高。抗氧化活性试验表明,经NKA-9树脂初步纯化后,绿豆皮黄酮对1,1-二苯基-2-三硝基苯肼自由基和·OH自由基有较强的清除能力。
The adsorption properties of macroporous resin NKA-9 to the flavonoids were studied via static adsorption experiments.Kinetics study indicated that the adsorption process could be best described by the pseudo-second-order model(R2>0.99),the isothermal adsorption followed the Langmuir model(R2>0.99).The best purification parameters optimized by dynamic adsorption and desorption tests were as follows:2 BV of 0.4 mg/mL flavonoids extract from mung bean hull(pH 3) was loaded onto the column at a flow rate of 2 BV/h and eluted with 2.3 BV of 70% ethanol(pH 5) at a flow rate of 2 BV/h,under these conditions,the purity of flavonids from mung bean hull was improved from 28.26% to75.74%,the recovery of flavonoids was increased from 24.56% to 64.91%.The results of high performance liquid chromatography(HPLC) analysis indicated that vitexin and isovitexin are the main component of flavonoids from mung bean hull,after purification,the purity of NKA-9 resin was improved significantly.Antioxidant activity tests showed that purified flavonoids from mung bean hull have a strong scavenging capacity to the 1,1-diphenyl-2-picrylhydrazyl(DPPH)radical and the hydroxyl radical.
The adsorption properties of macroporous resin NKA-9 to the flavonoids were studied via static adsorption experiments.Kinetics study indicated that the adsorption process could be best described by the pseudo-second-order model(R2>0.99),the isothermal adsorption followed the Langmuir model(R2>0.99).The best purification parameters optimized by dynamic adsorption and desorption tests were as follows:2 BV of 0.4 mg/mL flavonoids extract from mung bean hull(pH 3) was loaded onto the column at a flow rate of 2 BV/h and eluted with 2.3 BV of 70% ethanol(pH 5) at a flow rate of 2 BV/h,under these conditions,the purity of flavonids from mung bean hull was improved from 28.26% to75.74%,the recovery of flavonoids was increased from 24.56% to 64.91%.The results of high performance liquid chromatography(HPLC) analysis indicated that vitexin and isovitexin are the main component of flavonoids from mung bean hull,after purification,the purity of NKA-9 resin was improved significantly.Antioxidant activity tests showed that purified flavonoids from mung bean hull have a strong scavenging capacity to the 1,1-diphenyl-2-picrylhydrazyl(DPPH)radical and the hydroxyl radical.
引文
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[29]李斌,高凝轩,刘辉,等.大孔树脂纯化黑果腺肋花楸多酚的工艺优化[J].食品科学,2016,37(16):69-74.
[30]LI C,ZHENG Y Y,WANG X F,et al.Simultaneous separation and purification of flavonoids and oleuropein from Olea europaea L.(olive)leaves using macroporous resin[J].Journal of the Science of Food and Agriculture,2011,91(15):2826-2834.
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[32]ZHANG Y,LI S F,WU X W,et al.Macroporous resin adsorption for purification of flavonoids in Houttuynia cordata Thunb[J].Chinese Journel of Chemical Engineering,2007,15(6):872-876.
[33]骆党委,叶静,黄雅燕,等.AB-8大孔吸附树脂精制芦柑皮总黄酮及黄酮类化合物的分离[J].食品科学,2014,35(6):30-35.
[34]金慧鸣,郭红英,谭兴和,等.大孔吸附树脂-聚酰胺联用纯化茅岩莓总黄酮工艺优化[J].食品科学,2016,37(12):13-18.
[2]RAVISHANKAR D,RAJORA A K,GRECO F,et a1.Flavonoids as prospective compounds for anticancer therapy[J].International Journal of Biochemistry and Cell Biology,2013,45(12):2821-2831.
[3]OKOTH D A,CHENIA H Y,KOORBANALLY NA.Antibacterial and antioxidant activities of flavonoids from Lannea alata(Engl.)Engl.(Anacardiaceae)[J].Phytochemistry Letters,2013,6(3):476-481.
[4]FU Y,CHEN J,LI Y J,et al.Antioxidant and anti-inflammatory activities of six flavonoids separated from licorice[J].Food Chemistry,2013,141(2):1063-1071.
[5]MARAS J E,TALEGAWKAR S A,QIAO N,et al.Flavonoid intakes in the baltimore longitudinal study of aging[J].Journal of Food Composition and Analysis,2011,24(8):1103-1109.
[6]LUO J Q,CAI W X,Wu T,et al.Phytochemical distribution in hull and cotyledon of adzuki bean(Vigna angularis L.)and mung bean(Vigna radiate L.),and their contribution to antioxidant,anti-inflammatory and anti-diabetic activities[J].Food Chemistry,2016,201:350-360.
[7]张竞竞,曹冬冬,易建勇,等.绿豆皮水提液对大鼠高温条件下体内抗氧化能力的影响[J].核农学报,2014,28(6):1040-1046.
[8]CAO D D,LI H,YI J Y,et al.Antioxidant properties of the mung bean flavonoids on alleviating heat stress[J].PloS one,2011,6(6):1-9.
[9]LEE S,LEE J H,LEE H,et al.Effect of mung bean ethanol extract on pro-inflammtory cytokines in LPS stimulated macrophages[J].Food Science and Biotechnology,2011,20(2):519-524.
[10]朱文学,焦鲲鹏,罗磊,等.绿豆皮黄酮的超声波辅助水提工艺优化及抗氧化活性[J].食品科学,2015,36(16):12-17.
[11]SOTO M L,MOURE A,DOMINGUEZ H,et al Recovery,concentration and purification of phenolic compounds by adsorption:a review[J].Journal of Food Engineering,2011,105(1):1-27.
[12]DONG Y,ZHAO M M,SUN D X,et al.Absorption and desorption behaviour of the flavonoids from Glycyrrhiza glabra L.Leaf on macroporous adsorption resins[J].Food Chemistry,2015,168:538-545.
[13]安晓婷,周涛,李春阳,等.大孔树脂纯化蓝莓果渣多酚及其组成分析[J].食品科学,2013,34(20):1-6.
[14]王晓林,薛健飞,陈帅,等.大孔树脂法纯化锦灯笼宿萼总黄酮的工艺[J].食品科学,2014,35(14):58-61.
[15]熊利芝,李佳焱,王家坚,等.D-101大孔吸附树脂对黄花蒿黄酮的吸附热力学和动力学研究[J].离子交换与吸附,2014,30(4):334-339.
[16]陈莉华,肖斌,贺诚志,等.大孔吸附树脂对金银花叶茎藤总黄酮的吸附性能[J].天然产物研究与开发,2013,25:383-387.
[17]杨利敏,汪沣,杨自玲,等.苦荞黄酮在大孔树脂DM-2上的吸附特性的研究[J].食品研究与开发,2016,37(5):32-35.
[18]GAO B J,GAO Y C,LI Y B.Preparation and chelation adsorption property of composite chelating material poly(amidoxime)/SiO2towards heavy metal ions[J].Chemical Engineering Journal,2010,158(3):542-549.
[19]GAO Z P,YU Z F,YUE T L,et al.Adsorption isotherm,thermodynamics and kinetics studies of polyphenols separation from kiwifruit juice using adsorbent resin[J].Journal of Food Engineering,2013,116(1):195-201.
[20]RUAN X,ZHAN L M,GAO X X,et al.Separation and purification of flavonoid from taxus remainder extracts free of taxoids using polystyrene and polyamide resin[J].Journal of Separation Science,2013,36(12):1925-1934.
[21]董银卯.萌芽绿豆抗敏抗氧化活性物质分析及其作用机制研究[D].哈尔滨:哈尔滨工业大学,2014.
[22]LIU L X,SUN Y,LAURA T,et al.Determination of polyphenolic content and antioxidant activity of kudingcha made from Ilex kudingcha C.J.Tseng[J].Food Chemistry,2009,112(1):35-41.
[23]张禄捷,李荣,姜子涛.茼蒿叶中总黄酮的提取纯化及抗氧化活性分析[J].食品科学,2015,36(24):40-45.
[24]WAN P F,SHENG Z L,HAN Q,et al.Enrichment and purification of total flavonoids from Flos Populi extracts with macroporous resins and evaluation of antioxidant activities in vitro[J].Journal of Chromatography B Analytical Technologies in the Biomedical and life Sciences,2013,945/946(2):68-74.
[25]康家胜,方菊,魏凤玉,等.大孔树脂对竹叶黄酮的吸附平衡和动力学[J].化工进展,2011,30(10):2158-2162.
[26]王静,雷宏杰,岳珍珍,等.大孔树脂对红枣汁中棒曲霉素的吸附动力学[J].农业工程学报,2015,31(23):285-290.
[27]张媛,康尤丽,金天博,等.西藏雪莲总黄酮在大孔吸附树脂上的吸附动力学和热力学研究[J].离子交换与吸附,2016,32(4):358-367.
[28]熊利芝,王溶,田伟,等.大孔吸附树脂对杜仲叶总黄酮的吸附热力学和动力学研究[J].离子交换与吸附,2013,29(6):526-534.
[29]李斌,高凝轩,刘辉,等.大孔树脂纯化黑果腺肋花楸多酚的工艺优化[J].食品科学,2016,37(16):69-74.
[30]LI C,ZHENG Y Y,WANG X F,et al.Simultaneous separation and purification of flavonoids and oleuropein from Olea europaea L.(olive)leaves using macroporous resin[J].Journal of the Science of Food and Agriculture,2011,91(15):2826-2834.
[31]徐青,卢莹莹,辛建美,等.大孔树脂吸附分离海芦笋中黄酮类化合物工艺[J].食品科学,2011,32(2):115-119.
[32]ZHANG Y,LI S F,WU X W,et al.Macroporous resin adsorption for purification of flavonoids in Houttuynia cordata Thunb[J].Chinese Journel of Chemical Engineering,2007,15(6):872-876.
[33]骆党委,叶静,黄雅燕,等.AB-8大孔吸附树脂精制芦柑皮总黄酮及黄酮类化合物的分离[J].食品科学,2014,35(6):30-35.
[34]金慧鸣,郭红英,谭兴和,等.大孔吸附树脂-聚酰胺联用纯化茅岩莓总黄酮工艺优化[J].食品科学,2016,37(12):13-18.