大孔吸附树脂纯化东北岩高兰总黄酮
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摘要
依据东北岩高兰总黄酮的吸附和解吸能力,采用静态吸附和解吸实验对8种型号的大孔吸附树脂进行筛选。结果显示,AB-8型大孔吸附树脂对东北岩高兰总黄酮具有较好的吸附和解吸性能。经HPLC分析提取出的东北岩高兰主要有5种成分。进一步探究了总黄酮的纯化工艺,得到5种成分的最佳静态吸附解吸条件为:吸附平衡时间1.0 h,解吸溶剂为体积分数95%的乙醇,解吸平衡时间1.5 h。不同温度(25、30、35℃)下,AB-8型大孔吸附树脂对东北岩高兰不同成分的吸附等温线均符合Freundlich模型和Langmuir模型。5种成分的最佳动态吸附洗脱工艺条件为:上样液质量浓度为5 g/L,最大上样量400 mL,5倍柱体积(BV)的体积分数为20%的乙醇洗脱杂质,5倍BV的体积分数为95%的乙醇洗脱成分,洗脱流速3m L/min。在最佳实验条件下,东北岩高兰总黄酮的质量分数由纯化前的49.16%提高到纯化后的89.59%,表明AB-8型大孔吸附树脂能够有效纯化东北岩高兰。
Eight types of macroporous resins were compared via static adsorption-desorption methods with adsorption capacity and desorption capacity as dexes. Result indicated that AB-8 resin performed better adsorption and desorption properties to total flavonoids from Empetrum nigrum L. var. japonicum. There are five main components of Empetrum nigrum L. var. Japonicum extracted by HPLC analysis. Then, the purification process of total flavonoids was studied by static and dynamic adsorption-desorption experiments.The optimal static adsorption and desorption conditions for the five components were as follow: static adsorption equilibrium time was 1.0 h, desorption solvent was 95%(volume fraction) ethanol and desorption equilibrium time was 1.5 h. Adsorption isotherm of five components from Empetrum nigrum L. var.japonicum by AB-8 macroporous adsorption resin according with Freundlich model and Langmuir model at different temperatures(25、30、35 ℃). The optimal dynamic adsorption elution conditions for the five components were as follow:mass concentration of loading buffer was 5 g/L,the maximum sample volume was 400 mL, the impurities were washed by 5 BV 20%(volume fraction) ethanol, the components eluted with 95%(volume fraction) ethanol, elution volume was 5 BV, and elution flow rate was 3 mL/min. Finally,the purity of total flavonoids from Empetrum nigrum L. var. japonicum increased from 49.16% to 89.59%at the optimal experimental conditions. This experiment provides a reference for further study of Empetrum nigrum L. var. japonicum.
Eight types of macroporous resins were compared via static adsorption-desorption methods with adsorption capacity and desorption capacity as dexes. Result indicated that AB-8 resin performed better adsorption and desorption properties to total flavonoids from Empetrum nigrum L. var. japonicum. There are five main components of Empetrum nigrum L. var. Japonicum extracted by HPLC analysis. Then, the purification process of total flavonoids was studied by static and dynamic adsorption-desorption experiments.The optimal static adsorption and desorption conditions for the five components were as follow: static adsorption equilibrium time was 1.0 h, desorption solvent was 95%(volume fraction) ethanol and desorption equilibrium time was 1.5 h. Adsorption isotherm of five components from Empetrum nigrum L. var.japonicum by AB-8 macroporous adsorption resin according with Freundlich model and Langmuir model at different temperatures(25、30、35 ℃). The optimal dynamic adsorption elution conditions for the five components were as follow:mass concentration of loading buffer was 5 g/L,the maximum sample volume was 400 mL, the impurities were washed by 5 BV 20%(volume fraction) ethanol, the components eluted with 95%(volume fraction) ethanol, elution volume was 5 BV, and elution flow rate was 3 mL/min. Finally,the purity of total flavonoids from Empetrum nigrum L. var. japonicum increased from 49.16% to 89.59%at the optimal experimental conditions. This experiment provides a reference for further study of Empetrum nigrum L. var. japonicum.
引文
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[16]Liu Qingqing(刘清清),Yan Yizhu(阎怡竹),Yang Haixia(杨海霞),et al.The thermodynamic properties in the process of removing pyrethroid residue from honey using macroporous adsorption resins[J].Food and Fermentation Industries(食品与发酵工业),2016,42(12):57-61.
[17]Dong Haohao(董浩浩),Li Congju(李从举),Liu Tingyue(刘廷岳).et al.Kinetic and thermodynamic studies on absorption of anion exchange fiber in baicalin[J].Journal of Southwest China Normal Universit(Natural Science Editiony)(西南师范大学学报:自然科学版),2014,39(1):7-14.
[18]Zhang Shoujun(张守军),Wang Rongshen(王荣申),Lu Yan(卢燕),et al.Thermodynamic and kinetic characteristics of static adsorption of polyphenols from Toona sinensis seeds by macroporous resin[J].Chinese Traditional Patent Medicine(中成药),2016,38(11):2370-2374.
[19]Yang Jinyan(杨金燕),Guo Runqin(郭润勤),Xu Qing(徐清),et al.Enrichment and purification of total flavonoids from Emilia sonchifolia by macroporous adsorption resin[J].Journal of Chinese Medicinal Materials(中药材),2015,38(7):1517-1519.
[2]Kim K C,Lee I K,Kang K A,et al.Empetrum nigrum var.japonicum extract suppressesγ-ray radiation-induced cell damage via inhibition of oxidative stress[J].American Journal of Chinese Medicine,2011,39(1):161-170.
[3]Zhang Hongliang(张洪亮),Zhao Yujie(赵玉杰),Gao Dezhi(高德志).Necessity of protection of Empetrum nigrum germplasm resource in the Greater Xing'an Mountains,Inner Mongolia[J].Inner Mongolia Forestry Investigation and Design(内蒙古林业调查设计),2010,33(6):92-93.
[4]Kang Tingdi(康庭棣).Medicinal resources in daxinganling[M].Harbin:Harbin Publishing House(哈尔滨出版社),2001:294.
[5]Kim K C,Kang K A,Zhang R,et al.Risk reduction of ethyl acetate fraction of Empetrum nigrum var.japonicum via antioxidant properties against hydrogen peroxide-induced cell damage[J].Journal of Toxicology&Environmental Health,2009,72(21/22):1499-1508.
[6]Li Ruiming(李瑞明),Wang Zhenyue(王振月),Kang Yihua(康毅华),et al.Pharmacognostical studies on Empetrum nigrum[J].Central South Pharmacy(中南药学),2005,3(3):175-177
[7]Zhang Yulian(张玉莲),Mei Renqiang(梅任强),Liu Xi(刘熙),et al.Chemical constituents of Empetrum nigrum var.japonicum[J].Chinese Traditional and Herbal Drugs(中草药),2014,45(16):2293-2298.
[8]Zhao Ming(赵明),Huang Shulei(黄淑蕾),Wang Dan(王丹),et al.Chalcones from Empetrum nigrum var.japonicum[J].Chinese Traditional and Herbal Drugs(中草药),2016,47(24):4318-4321.
[9]Huang Shulei(黄淑蕾),Zhao Ming(赵明),Li Jun(李军),et al.Chemical constituents of Empetrum nigrum L.var.japonicum[J].Journal of Qiqihar University(Natural Science Edition)(齐齐哈尔大学学报:自然科学版),2016,32(4):54-55.
[10]Song Manling(宋漫玲),Tao Junyu(陶俊宇),Yang Jian(杨剑),et al.Study on separation and purification of total flavonoids from Polygonum hydropiper Linn.by macroporous resin[J].Chinese Journal of Information on TCM(中国中医药信息杂志),2018,25(1):74-78.
[11]Zhao Jiahong(赵家洪),Yan Xin(焉鑫),Wang Biying(王碧莹),et al.Preliminary enrichment and separation of gallic acid from Chebulae Fructus by macroporous resins[J].Fine Chemicls(精细化工),2018,35(4):597-602.
[12]Yan Youyu(鄢又玉),Xia Ting(夏婷),Zhang Yu(张育),et al.Systematic investigation on AlCl3 colorimetric determination of total flavonoids from pyracantha fortuneana fruit[J].Food Research and Development(食品研究与开发),2015,36(5):89-94.
[13]Ye Chun(叶春),Xu Lijuan(徐丽娟),Yang Genqin(杨根勤),et al.Determination and identification of flavonoids in leaves of houttuynia cordata thumb[J].Food Research and Development(食品研究与开发),2007,24(9):542-546.
[14]Liu Dongyan(刘冬彦),Shi Xiaofeng(石晓峰),Hu Pengbin(胡鹏斌),et al.Optimization of enrichment and purification of total flavonoids from pine needles of Cedrus deodara by macroporous adsorption resin[J].Chinese Traditional Patent Medicine(中成药),2017,39(2):308-311.
[15]Fan Qin(樊秦),Xia Pengfei(夏鹏飞),Peng Xuejing(彭雪晶),et al.Enrichment of atractylenolide I and atractylenolideⅡfrom Codonopsispilosula with macroporous resin[J].Natural Product Research and Development(天然产物研究与开发),2017,29(9):1602-1607.
[16]Liu Qingqing(刘清清),Yan Yizhu(阎怡竹),Yang Haixia(杨海霞),et al.The thermodynamic properties in the process of removing pyrethroid residue from honey using macroporous adsorption resins[J].Food and Fermentation Industries(食品与发酵工业),2016,42(12):57-61.
[17]Dong Haohao(董浩浩),Li Congju(李从举),Liu Tingyue(刘廷岳).et al.Kinetic and thermodynamic studies on absorption of anion exchange fiber in baicalin[J].Journal of Southwest China Normal Universit(Natural Science Editiony)(西南师范大学学报:自然科学版),2014,39(1):7-14.
[18]Zhang Shoujun(张守军),Wang Rongshen(王荣申),Lu Yan(卢燕),et al.Thermodynamic and kinetic characteristics of static adsorption of polyphenols from Toona sinensis seeds by macroporous resin[J].Chinese Traditional Patent Medicine(中成药),2016,38(11):2370-2374.
[19]Yang Jinyan(杨金燕),Guo Runqin(郭润勤),Xu Qing(徐清),et al.Enrichment and purification of total flavonoids from Emilia sonchifolia by macroporous adsorption resin[J].Journal of Chinese Medicinal Materials(中药材),2015,38(7):1517-1519.
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