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作者王露(2019)在《废次桑叶中高纯异槲皮苷提制工艺及其过程研究》一文中研究指出:作为“药食同源”物,桑叶药理价值极高,因生产经营或加工技术等原因,存在利用率低等问题,导致高附加值的成份流失,造成桑资源浪费。本文以废次桑叶为原料,将水热反应引入天然产物提取技术中,开展提制高附加值天然活性成份异槲皮苷等研究,变废为宝,实现桑资源增值开发的高值利用,符合国家国民健康与资源利用战略。为提高桑叶中异槲皮苷等活性成份的有效溶出,采用水热反应方法,以异槲皮苷溶浸效率为评价指标,探讨水热时间、料液比、水热温度和乙醇体积分数等因素对异槲皮苷溶出的影响,经响应曲面法优化获得水热辅助醇提取桑叶中异槲皮苷的适宜参数,并开展提取物体外抗氧化作用研究;运用SEM(电镜扫描)、BET(比表面积)和FTIR(红外光谱)等手段,分析表征水热反应前后桑叶植物组织的物相结构及组分变化,探究水热降解植物组织的性能。为进一步揭示异槲皮苷溶浸的制约因素及传质规律,通过计算传质系数k、活化能Ea、相对萃余率y及有效扩散系数Ds等动力学参数,开展异槲皮苷溶浸的动力学研究;分析异槲皮苷溶浸的扩散过程,建立异槲皮苷的内扩散模型,获得异槲皮苷扩散速率常数。为获得高纯度异槲皮苷单体,采用制备色谱方法,开展流动相组成及比列、流速和进样量等条件比选,获得异槲皮苷分离、纯化的适宜条件,并评价提取物经济收益。结论如下:(1)采用响应曲面法优化获得水热反应辅助醇法提取异槲皮苷的适宜参数为:以体积分数为57%的乙醇为提取剂,桑叶质量(g)与乙醇体积(v)之比为1:7,在水热温度154℃、水热解80min后,5g桑叶提取异槲皮苷3.64mg·g-1,是乙醇提法的51倍。响应曲面法拟合所得异槲皮苷溶浸方程R2=0.9582,F=22.91,P<0.0001,表明模型显著性极高,可用;F值检验可知,影响桑叶中异槲皮苷含量的因素顺序分别为:水热时间>水热温度>料液比>乙醇体积分数,且水热时间和水热温度的交互作用对异槲皮苷溶浸量影响显著。桑叶提取液对DPPH的清除率、超氧阴离子清除率、脂质过氧化抑制率、还原能力的实验表明,桑叶提取液在较低浓度0.02mg·mL-1表现出抗氧化能力,且在0.02mg·mL-10.1mg·mL-1范围内呈现正相关。(2)红外分光谱分析表明,水热反应有助于桑叶中C-O、C-H、>C=C<键断裂,促进桑叶木质素中苯基丙烷结构单元分解;扫描电镜结果显示经水热解后的桑叶组织间出现孔洞且孔隙较大;BET结果表明经水热解后的底物比表面积是未经水热反应的桑叶底物的1.8倍左右;表明水热反应能有效降解桑叶植物纤维组织,有利于天然活性成份溶出。粒子扩散模模型表明,异槲皮苷的扩散存在渗透、内部扩散和边界扩散三个过程,扩散速率常数k随着边界层厚度增加而变小,其边界层厚度常数C依次为CⅠ<CⅡ<CⅢ。(3)Fick第二定律获得的桑叶异槲皮苷溶浸动力学模型表明,在温度为120℃160℃时,速率常数k为0.0157min-10.0301min-1,表观活化能Ea=27.22kJ·mol-1,指前因子A为0.0164min-1,表观活化能越小,有利于反应的进行;有效扩散系数Ds为0.52×10-4mm2·min-10.99×10-4mm2·min-1,且随温度升高而增大;萃余率y随着温度升高而减少,在154℃下萃余率最小为9.75%,此时异槲皮苷的溶浸率最为91.25%;通过热力学分析求出ΔGm在-4.3743kJ·mol-1-1.2582kJ·mol-1<0,ΔHm=34.907kJ·mol-1>0,ΔSm=92.47J·mol-1>0,表明水热辅助醇提取异槲皮苷过程是吸热熵增的过程。(4)采用制备色谱分离纯化获得异槲皮苷,分离纯化适宜条件为:V乙腈:V水=20:80,进样量10mL,流速20mL·min-1,异槲皮苷分离度为1.74,视为完全分离,纯度较高,同时可得到绿原酸、芦丁和紫云英苷,其分离度均大于1.5;经冷冻干燥后,制得异槲皮苷纯度为98.78%,含率为取粗含量的4.26%;同时制得绿原酸纯度为99.47%,含率为粗提物的6.74%,芦丁纯度为98%、含率为粗提物的1.36%,紫云英苷纯度为98%,含率为粗提物的0.35%,为桑叶资源多元产品开发提供单体或复合物原料支撑。
Abstract
zuo wei “yao shi tong yuan ”wu ,sang xie yao li jia zhi ji gao ,yin sheng chan jing ying huo jia gong ji shu deng yuan yin ,cun zai li yong lv di deng wen ti ,dao zhi gao fu jia zhi de cheng fen liu shi ,zao cheng sang zi yuan lang fei 。ben wen yi fei ci sang xie wei yuan liao ,jiang shui re fan ying yin ru tian ran chan wu di qu ji shu zhong ,kai zhan di zhi gao fu jia zhi tian ran huo xing cheng fen yi hu pi gan deng yan jiu ,bian fei wei bao ,shi xian sang zi yuan zeng zhi kai fa de gao zhi li yong ,fu ge guo jia guo min jian kang yu zi yuan li yong zhan lve 。wei di gao sang xie zhong yi hu pi gan deng huo xing cheng fen de you xiao rong chu ,cai yong shui re fan ying fang fa ,yi yi hu pi gan rong jin xiao lv wei ping jia zhi biao ,tan tao shui re shi jian 、liao ye bi 、shui re wen du he yi chun ti ji fen shu deng yin su dui yi hu pi gan rong chu de ying xiang ,jing xiang ying qu mian fa you hua huo de shui re fu zhu chun di qu sang xie zhong yi hu pi gan de kuo yi can shu ,bing kai zhan di qu wu ti wai kang yang hua zuo yong yan jiu ;yun yong SEM(dian jing sao miao )、BET(bi biao mian ji )he FTIR(gong wai guang pu )deng shou duan ,fen xi biao zheng shui re fan ying qian hou sang xie zhi wu zu zhi de wu xiang jie gou ji zu fen bian hua ,tan jiu shui re jiang jie zhi wu zu zhi de xing neng 。wei jin yi bu jie shi yi hu pi gan rong jin de zhi yao yin su ji chuan zhi gui lv ,tong guo ji suan chuan zhi ji shu k、huo hua neng Ea、xiang dui cui yu lv yji you xiao kuo san ji shu Dsdeng dong li xue can shu ,kai zhan yi hu pi gan rong jin de dong li xue yan jiu ;fen xi yi hu pi gan rong jin de kuo san guo cheng ,jian li yi hu pi gan de nei kuo san mo xing ,huo de yi hu pi gan kuo san su lv chang shu 。wei huo de gao chun du yi hu pi gan chan ti ,cai yong zhi bei se pu fang fa ,kai zhan liu dong xiang zu cheng ji bi lie 、liu su he jin yang liang deng tiao jian bi shua ,huo de yi hu pi gan fen li 、chun hua de kuo yi tiao jian ,bing ping jia di qu wu jing ji shou yi 。jie lun ru xia :(1)cai yong xiang ying qu mian fa you hua huo de shui re fan ying fu zhu chun fa di qu yi hu pi gan de kuo yi can shu wei :yi ti ji fen shu wei 57%de yi chun wei di qu ji ,sang xie zhi liang (g)yu yi chun ti ji (v)zhi bi wei 1:7,zai shui re wen du 154℃、shui re jie 80minhou ,5gsang xie di qu yi hu pi gan 3.64mg·g-1,shi yi chun di fa de 51bei 。xiang ying qu mian fa ni ge suo de yi hu pi gan rong jin fang cheng R2=0.9582,F=22.91,P<0.0001,biao ming mo xing xian zhe xing ji gao ,ke yong ;Fzhi jian yan ke zhi ,ying xiang sang xie zhong yi hu pi gan han liang de yin su shun xu fen bie wei :shui re shi jian >shui re wen du >liao ye bi >yi chun ti ji fen shu ,ju shui re shi jian he shui re wen du de jiao hu zuo yong dui yi hu pi gan rong jin liang ying xiang xian zhe 。sang xie di qu ye dui DPPHde qing chu lv 、chao yang yin li zi qing chu lv 、zhi zhi guo yang hua yi zhi lv 、hai yuan neng li de shi yan biao ming ,sang xie di qu ye zai jiao di nong du 0.02mg·mL-1biao xian chu kang yang hua neng li ,ju zai 0.02mg·mL-10.1mg·mL-1fan wei nei cheng xian zheng xiang guan 。(2)gong wai fen guang pu fen xi biao ming ,shui re fan ying you zhu yu sang xie zhong C-O、C-H、>C=C<jian duan lie ,cu jin sang xie mu zhi su zhong ben ji bing wan jie gou chan yuan fen jie ;sao miao dian jing jie guo xian shi jing shui re jie hou de sang xie zu zhi jian chu xian kong dong ju kong xi jiao da ;BETjie guo biao ming jing shui re jie hou de de wu bi biao mian ji shi wei jing shui re fan ying de sang xie de wu de 1.8bei zuo you ;biao ming shui re fan ying neng you xiao jiang jie sang xie zhi wu qian wei zu zhi ,you li yu tian ran huo xing cheng fen rong chu 。li zi kuo san mo mo xing biao ming ,yi hu pi gan de kuo san cun zai shen tou 、nei bu kuo san he bian jie kuo san san ge guo cheng ,kuo san su lv chang shu ksui zhao bian jie ceng hou du zeng jia er bian xiao ,ji bian jie ceng hou du chang shu Cyi ci wei CⅠ<CⅡ<CⅢ。(3)Fickdi er ding lv huo de de sang xie yi hu pi gan rong jin dong li xue mo xing biao ming ,zai wen du wei 120℃160℃shi ,su lv chang shu kwei 0.0157min-10.0301min-1,biao guan huo hua neng Ea=27.22kJ·mol-1,zhi qian yin zi Awei 0.0164min-1,biao guan huo hua neng yue xiao ,you li yu fan ying de jin hang ;you xiao kuo san ji shu Dswei 0.52×10-4mm2·min-10.99×10-4mm2·min-1,ju sui wen du sheng gao er zeng da ;cui yu lv ysui zhao wen du sheng gao er jian shao ,zai 154℃xia cui yu lv zui xiao wei 9.75%,ci shi yi hu pi gan de rong jin lv zui wei 91.25%;tong guo re li xue fen xi qiu chu ΔGmzai -4.3743kJ·mol-1-1.2582kJ·mol-1<0,ΔHm=34.907kJ·mol-1>0,ΔSm=92.47J·mol-1>0,biao ming shui re fu zhu chun di qu yi hu pi gan guo cheng shi xi re shang zeng de guo cheng 。(4)cai yong zhi bei se pu fen li chun hua huo de yi hu pi gan ,fen li chun hua kuo yi tiao jian wei :Vyi jing :Vshui =20:80,jin yang liang 10mL,liu su 20mL·min-1,yi hu pi gan fen li du wei 1.74,shi wei wan quan fen li ,chun du jiao gao ,tong shi ke de dao lu yuan suan 、lu ding he zi yun ying gan ,ji fen li du jun da yu 1.5;jing leng dong gan zao hou ,zhi de yi hu pi gan chun du wei 98.78%,han lv wei qu cu han liang de 4.26%;tong shi zhi de lu yuan suan chun du wei 99.47%,han lv wei cu di wu de 6.74%,lu ding chun du wei 98%、han lv wei cu di wu de 1.36%,zi yun ying gan chun du wei 98%,han lv wei cu di wu de 0.35%,wei sang xie zi yuan duo yuan chan pin kai fa di gong chan ti huo fu ge wu yuan liao zhi cheng 。
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论文作者分别是来自重庆工商大学的王露,发表于刊物重庆工商大学2019-06-28论文,是一篇关于桑叶论文,异槲皮苷论文,水热反应论文,动力学分析论文,重庆工商大学2019-06-28论文的文章。本文可供学术参考使用,各位学者可以免费参考阅读下载,文章观点不代表本站观点,资料来自重庆工商大学2019-06-28论文网站,若本站收录的文献无意侵犯了您的著作版权,请联系我们删除。
标签:桑叶论文; 异槲皮苷论文; 水热反应论文; 动力学分析论文; 重庆工商大学2019-06-28论文;