离子液体超声辅助提取香叶总黄酮及其抗氧化性研究
第４３卷第４期 ２０１８年４月
中国调味品
Ｃｈｉｎａ Ｃｏｎｄｉｍｅｎｔ 基础研究
离子液体超声辅助提取香叶总黄酮 及其抗氧化性研究
钟方丽 ，金龙哲。，王晓林 ＇ 谷 （１．吉林化工学院化学与制药工程学院，吉林吉林１３２０２２；２．延边朝鲜族自治州 农业科学院，吉林延吉１３３００１）
摘要：探索离子液体超声辅助提取香叶总黄酮的工艺条件及其体外抗氧化活性。以香叶总黄酮提取率 为考察指标，采用单因素及正交试验对香叶总黄酮的提取工艺进行考察；应用紫外一分光光度法测定了 香叶总黄酮对ＤＰＰＨ·的清除率。试验结果说明香叶总黄酮的最佳提取工艺条件为：提取溶剂为４Ｏ 乙醇水溶液，料液比为１：５０、离子液体为氯化一１一丁基一３一甲基咪唑，离子液体浓度为０．３５ ｍｏｌ／Ｌ，提取 水浴温度为６５℃、提取时间为３ ｈ、超声波频率为９Ｏ ｗ，在上述最佳提取工艺参数下，离子液体超声辅 助提取香叶总黄酮的提取率可以达到１０９．７９ ｍｇ／ｇ。体外清除自由基试验结果表明香叶总黄酮清除 ＤＰＰＨ·的ＩＣ５ｏ为０．２３６０ ｍｇ／ｍＬ，说明香叶总黄酮具有显著的体外抗氧化活性。研究结果为香叶的进 一步开发利用提供了依据。 关键词：香叶；总黄酮；离子液体；提取 中图分类号：ＴＳ２６４．３ 文献标志码：Ａ ｄｏｉ：１０．３９６９／ｊ．ｉｓｓｎ．１０００—９９７３．２０１８．０４．０１４ 文章编号：１０００－９９７３（２０１８）０４—００６９—０６ Ｓｔｕｄｙ ｏｎ Ｐｒｏｃｅｓｓ ｏｆ Ｉｏｎｉｃ Ｌｉｑｕｉｄ－ｂａｓｅｄ Ｕｌｔｒａｓｏｎｉｃ。ａｓｓｉｓｔｅｄ Ｅｘｔｒａｃｔｉｏｎ ｏｆ Ｔｏｔａｌ Ｆｌａｖｏｎｏｉｄｓ ｆｒＯｍ Ｐｅｌａｒｇｏｎｉｕｍ ｇｒａｖｅｏｌｅｎｓ ａｎｄ Ｔｈｅｉｒ声ｎｔｉｏｘｉｄａｎｔ Ｅｆｆｅｃｔ ＺＨＯＮＧ Ｆａｎｇ－ｌｉ ，ＪＩＮ Ｌｏｎｇ－ｚｈｅ。，ＷＡＮＧ Ｘｉａｏ－ｌｉｎ¨，ＧＵ Ｙｕｅ （１．Ｓｃｈｏｏｌ ｏｆ Ｃｈｅｍｉｓｔｒｙ ａｎｄ Ｐｈａｒｍａｃｅｕｔｉｃａｌ Ｅｎｇｉｎｅｅｒｉｎｇ，Ｊｉｌｉｎ Ｉｎｓｔｉｔｕｔｅ ｏｆ Ｃｈｅｍｉｃａｌ Ｔｅｃｈｎｏｌｏｇｙ， Ｊｉｌｉｎ １３２０２２，Ｃｈｉｎａ；２．Ｙａｎｂｉａｎ Ａｃａｄｅｍｙ ｏｆ Ａｇｒｉｃｕｌｔｕｒａｌ Ｓｃｉｅｎｃｅｓ，Ｙａｎｊｉ １３３００１，Ｃｈｉｎａ） Ａｂｓｔｒａｃｔ，Ｔｏ ｓｔｕｄｙ ｔｈｅ ｅｘｔｒａｃｔｉｏｎ ｔｅｃｈｎｏｌｏｇｙ ｏｆ ｔｏｔａｌ ｆｌａｖｏｎｏｉｄｓ ｆｒｏｍ Ｐｅｌａｒｇｏｎｉｕｍ ｇｒａｖｅｏｌｅｎｓ ｗｉｔｈ ｉｏｎｉｃ ｌｉｑｕｉｄ—ｂａｓｅｄ ｕｌｔｒａｓｏｎｉｃ－ａｓｓｉｓｔｅｄ ａｎｄ ｔｈｅｉｒ ａｎｔｉｏｘｉｄａｎｔ ａｂｉｌｉｔｙ，ｕｓｉｎｇ ｅｘｔｒａｃｔｉｏｎ ｒａｔｅ ｏｆ ｔｏｔａｌ ｆｌａｖｏｎｏｉｄｓ ａｓ ｔｈｅ ｒｅｆｅｒｅｎｃｅ ｉｎｄｅｘ，ｔｈｅ ｓｉｎｇｌｅ ｆａｃｔｏｒ ａｎｄ ｏｒｔｈｏｇｏｎａｌ ｅｘｐｅｒｉｍｅｎｔｓ ａｒｅ ａｐｐｌｉｅｄ ｔｏ ｏｐｔｉｍｉｚｅ ｔｈｅ ｅｘｔｒａｃｔｉｏｎ ｔｅｃｈｎｏｌｏｇｙ ｏｆ ｔｏｔａｌ ｆｌａｖｏｎｏｉｄｓ ｆｒｏｍ Ｐｅｌａｒｇｏｎｉｕｍ ｇｒａｖｅｏｌｅｎｓ．Ｔｈｅ ｒｅｍｏｖａｌ ｒａｔｅ ｏｆ ｔｏｔａｌ ｆｌａｖｏｎｏｉｄｓ ｆｒｏｍ Ｐｅｌａｒｇｏｎｉｕｍ ｇｒａｖｅｏｌｅｎｓ ｏｎ ＤＰＰＨ·ｉｓ ｄｅｔｅｒｍｉｎｅｄ ｂｙ ＵＶ－ｓｐｅｃｔｒｏｐｈｏｔｏｍｅｔｒｙ．Ｔｈｅ ｒｅｓｕｌｔｓ ｓｈｏｗ ｔｈａｔ ｔｈｅ ｏｐｔｉｍｕｍ ｅｘｔｒａｃｔｉｏｎ ｔｅｃｈｎｏｌｏｇｙ ｏｆ ｔｏｔａｌ ｆｌａｖｏｎｏｉｄｓ ｆｒｏｍ Ｐｅｌａｒｇｏｎｉｕｒｎ ｇｒａｖｅｏｌｅｎｓ ｗｉｔｈ ｉｏｎｉｃ ｌｉｑｕｉｄ－ｂａｓｅｄ ｕｌｔｒａｓｏｎｉｃ－ａｓｓｉｓｔｅｄ ｉｓ ｏｂｔａｉｎｅｄ ａｓ ｆｏｌｌｏｗｓ：ｔｈｅ ｅｘｔｒａｃｔｉｏｎ ｓｏｌｖｅｎｔ ｉｓ ４０ ｅｔｈａｎｏｌ
收稿日期：２Ｏ１７—１０－１８ ＊通讯作者 作者简介：钟方丽（１９７Ｏ一），女，山东安丘人，教授，硕士生导师，博士。主要从事天然产物化学成分的分离与生物活性方面的研究｝ 王晓林（１９６９一），男，山东五莲人，副教授，硕士，主要从事天然产物有效成分的提取、纯化及药物的研制与开发方面的研究。 ’ 一６９— 第４３卷第４期 ２０１８年４月
中国调味品 Ｃｈｉｎａ Ｃｏｎｄｉｍｅｎｔ 基础研究
ａｑｕｅｏｕｓ ｓｏｌｕｔｉｏｎ，ｔｈｅ ｒａｔｉｏ ｏｆ ｒａｗ ｍａｔｅｒｉａｌ ａｎｄ ｓｏｌｖｅｎｔ ｉｓ １：５０，ｔｈｅ ｉｏｎｉｃ ｌｉｑｕｉｄ ｉｓ ｃｈｌｏｒｉｎａｔｅｄ—ｌ—ｂｕｔｙｌ一 ３一ｍｅｔｈｙｌ ｉｍｉｄａｚｏｌｅ，ｔｈｅ ｉｏｎｉｃ ｌｉｑｕｉｄ ｃｏｎｃｅｎｔｒａｔｉｏｎ ｉｓ ０．３５ ｍｏｌ／Ｌ，ｔｈｅ ｔｅｍｐｅｒａｔｕｒｅ ｏｆ ｗａｔｅｒ ｂａｔｈ ｉｓ ６５℃，ｔｈｅ ｅｘｔｒａｃｔｉｏｎ ｔｉｍｅ ｉｓ ３ ｈ，ａｎｄ ｔｈｅ ｕｌｔｒａｓｏｎｉｃ ｆｒｅｑｕｅｎｃｙ ｉｓ ９０ Ｗ．Ｉｎ ｔｈｅ ａｂｏｖｅ ｏｐｔｉｍｕｍ ｅｘｔｒａｃｔｉｏｎ ｐｒｏｃｅｓｓ ｐａｒａｍｅｔｅｒｓ，ｔｈｅ ｅｘｔｒａｃｔｉｏｎ ｅｆｆｉｃｉｅｎｃｙ ｏｆ ＴＦ ｉｓ １０９．７９ ｍｇ／ｇ．Ｔｈｅ ｒｅｓｕｌｔｓ ｏｆ ｓｃａｖｅｎｇｉｎｇ ｆｒｅｅ ｒａｄｉｃａｌｓ ｉｎ ｖｉｔｒｏ ｓｈｏｗ ｔｈａｔ ｔｈｅ ＩＣ５０ ｏｆ ｓｃａｖｅｎｇｉｎｇ ＤＰＰＨ·ｏｆ ｔｏｔａｌ ｆｌａｖｏｎｏｉｄｓ ｆｒｏｍ Ｐｅｌａｒｇｏｎｉｕｍ ｇｒａｖｅｏｌｅｎｓ ｉｓ ０．２３６０ ｍｇ／ｍＬ．Ｔｈｅ ｒｅｓｕｌｔｓ ｓｈｏｗ ｔｈａｔ ｔｈｅ ｔｏｔａｌ ｆｌａｖｏｎｏｉｄｓ ｆｒｏｍ Ｐｅｌａｒｇｏｎｉｕｍ ｇｒａｖｅｏｌｅｎｓ ｈａｖｅ ｓｉｇｎｉｆｉｃａｎｔ ａｎｔｉｏｘｉｄａｎｔ ａｃｔｉｖｉｔｙ ｉｎ ｖｉｔｒｏ．Ｔｈｅ ｒｅｓｕｌｔｓ ｈａｖｅ ｐｒｏｖｉｄｅｄ ａ ｂａｓｉｓ ｆｏｒ ｆｕｒｔｈｅｒ ｄｅｖｅｌｏｐｍｅｎｔ ａｎｄ ｕｔｉｌｉｚａｔｉｏｎ ｏｆ Ｐｅｌａｒｇｏｎｉｕｍ ｇｒａｖｅｏｌｅｎｓ． Ｋｅｙ ｗｏｒｄｓ：Ｐｅｌａｒｇｏｎｉｕｍ ｇｒａｖｅｏｌｅｎｓ Ｌ．；ｔｏｔａｌ ｆｌａｖｏｎｏｉｄｓ；ｉｏｎｉｃ ｌｉｑｕｉｄ；ｅｘｔｒａｃｔｉｏｎ
香叶为植物香叶天竺葵的茎叶，我国各地均有栽 培，全草具有清新芳香气味，香叶含有芳香挥发油，其 主要成分是芳樟醇、丁香油酚、香茅醇、桉叶素等［１ ］。 香叶作为调味料常用于汤类或肉类烹调时的调味，也 是西餐常用芳香调味料之一，香叶除了作为调味品使 用外，尚具有祛风除湿、行气止痛、杀虫之功效［３］。香 叶除含有芳香挥发油外，还含有大量的黄酮类成分［４］， 而黄酮类化合物具有清除自由基、提高免疫力、抗衰老 等多种生理活性，在药品、饮料、食品领域应用广 泛Ｌ５ ］。离子液体是由有机阳离子和有机或无机阴离 子组成的在室温下呈液体的有机离子体系［７］。由于离 子液体具有挥发性小、性质稳定、溶解能力强等独特的 物理化学性质，现已在天然产物活性成分提取领域有 所应用［８ 。。，与传统的有机溶剂相比，离子液体具有 绿色环保、热稳定性好、不挥发、不易燃烧等特点，被认 为是代替传统有机溶剂更环保的溶剂口 。因此，本研 究采用离子液体辅助超声技术，以香叶总黄酮提取率 为评价指标，通过单因素和正交试验优化了香叶总黄 酮的提取工艺条件，并探索了香叶对ＤＰＰＨ·的清除 活性，为香叶的深入开发提供了试验依据。 １ 材料与方法 １．１材料与试剂 香叶，购于毫州康民中药材批发行；芦丁，中国食 品药品检定研究院（供含量测定用）；溴化一１一丁基一３一甲 基咪唑、氯化一１一丁基一３一甲基咪唑、ｌ－丁基一３一甲基咪唑 硝酸盐、１一丁基一３一甲基咪唑硫酸氢盐、卜丁基一３一甲基咪 唑四氟硼酸盐，上海成捷化学有限公司；纤维素酶，北 京鼎国昌盛生物技术有限责任公司；维生素Ｃ，天津市 永大化学试剂有限公司；ＤＰＰＨ·，上海如吉生物科技 有限公司；硝酸铝、氢氧化钠、亚硝酸钠、无水乙醇（均 一７０一 为分析纯），天津市永大化学试剂有限公司；水（重蒸馏 水）；其余所用试剂（均为化学纯）。 １．２仪器与设备 ＴＵ一１９５０紫外可见分光光度计 北京普析通用 仪器有限责任公司；ＲＥ一５２ＡＡ旋转蒸发器上海亚荣 生化仪器厂；ｗ５—１００ＳＰ恒温水浴锅 上海申生科技 有限公司；ＦＡ一３２０４Ｂ电子分析天平 上海精密科学 仪器有限公司；ＳＨＢ—ＩｌＩＡ型循环水式真空泵郑州长 城科工贸有限公司；ＤＨＧ一９０７６Ａ电热鼓风干燥器 上海精密实验设备有限公司；ＫＱ１１８超声波清洗器 昆山市超声仪器有限公司。 １．３试验方法 １．３．１标准曲线的制备 称取干燥至恒重的芦丁１０ ｍｇ，精密称定，置于 ５Ｏ ｍＬ容量瓶中，加入５０ 乙醇水溶液，超声使其溶 解。定容，摇匀，使之成为每１ ｍＬ含０．１８５６ ｍｇ的芦 丁对照品溶液，备用。在７个容量瓶中分别放人芦丁 对照品溶液１２．０，１０．０，８．０，６．０，４．０，２．０，１．０ ｍＬ，于 ３０℃水浴条件下，分别加入０．３ ｍＬ的５ ９／６ ＮａＮＯ２溶 液，轻轻振摇２ ｍｉｎ，然后静置６ ｒａｉｎ，向每个容量瓶中 加入浓度为１Ｏ 的硝酸铝溶液０．３ ｍＬ，慢慢摇晃 ２ ｍｉｎ，然后静置６ ｍｉｎ，再向每个容量瓶中加入浓度为 ４ ９，６的氢氧化钠溶液２．０ ｍＬ，用５Ｏ 乙醇定容，摇匀，放 置１５ ｒａｉｎ，以相应对照品溶液为空白，按照紫外可见分 光光度法，于５１０ ｎｉｎ波长处测吸光度［１引。以浓度Ｃ （ｍｇ／ｍＬ）为横坐标，吸光度值Ａ为纵坐标，进行直线 回归，绘制标准曲线，芦丁的线性范围为０．００７４２４～ ０．０８９０９ ｍｇ／ｍＬ，回归方程：Ａ一１０．３０８８Ｃ一０．０４４８４， Ｒ一０．９９９３。 １．３．２样品含量测定 精密吸取香叶提取液适量于２５ ｍＬ容量瓶中，按
白骨壤叶总黄酮的超声辅助提取及抗氧化活性研究
白骨壤叶总黄酮的超声辅助提取及抗氧化活性研究夏杏洲;韩维栋;杨维;郭远鑫;王维民;谌素华【期刊名称】《食品科学》【年(卷),期】2012(033)014【摘要】在单因素试验基础上，采用响应面分析法研究乙醇体积分数、固液比、超声功率和提取时间4个白骨壤叶总黄酮超声辅助提取因素，并比较白骨壤叶总黄酮的体外抗氧化作用。
结果表明：白骨壤叶黄酮超声提取的最佳工艺条件为以粒度40-60甘的白骨壤叶干粉为原料、乙醇体积分数64．39％、固液比1：28．20（g／mL）、提取功率293．63W、提取时间40．00min，该条件下白骨壤叶中总黄酮提取率为4．185％。
白骨壤叶总黄酮体外清除羟自由基、超氧阴离子自山基和1，1-二苯基苦基苯肼（DPPH）自由基的IC50值分别0．232、0．829、23．692mg／L，其清除3种自由基的能力均高于VC。
【总页数】5页(P20-24)【作者】夏杏洲;韩维栋;杨维;郭远鑫;王维民;谌素华【作者单位】广东海洋大学食品科技学院,广东湛江524088／华南理工大学轻工与食品学院,广东广州510640;广东海洋大学农学院,广东湛江524088;广东海洋大学食品科技学院,广东湛江524088;广东海洋大学食品科技学院,广东湛江524088;广东海洋大学食品科技学院,广东湛江524088;广东海洋大学食品科技学院,广东湛江524088【正文语种】中文【中图分类】R284.2【相关文献】1.白骨壤叶黄酮提取及抗氧化活性研究 [J], 孙国强;赵丰丽;刘哲瑜;戴旭青;叶日娜2.黄花草总黄酮超声辅助提取工艺优化及抗氧化活性研究 [J], 许建本; 苏秀芳; 黄妹胶3.超声辅助提取款冬总黄酮工艺及抗氧化活性研究 [J], 陈苏丹; 汪亚祺; 李秀珍; 李学强4.响应面法优化超声辅助提取玉竹药渣总黄酮工艺及抗氧化活性研究 [J], 王萍;王宇鹤;赖普辉5.响应面法优化超声辅助提取肉豆蔻总黄酮工艺及其抗氧化活性研究 [J], 卓微伟;李凤;胡君因版权原因，仅展示原文概要，查看原文内容请购买。
超声辅助离子液体和酶解法提取羊肚菌多糖及其抗氧化活性研究
超声辅助离子液体和酶解法提取羊肚菌多糖及其抗氧化活性研
究
贾庆超
【期刊名称】《粮食与油脂》
【年(卷),期】2024(37)3
【摘要】分别采用超声辅助离子液体法(L法)和酶解法(M法)提取羊肚菌多糖。
以多糖得率为指标,在单因素试验的基础上通过响应面法优化提取工艺,并研究羊肚菌多糖的抗氧化活性。
结果表明:L法最佳提取工艺为料液比1∶26(g/mL)、超声温度55℃、离子液体体积1.6 mL、超声时间32 min,多糖得率为
18.10%±0.25%;M法最佳提取工艺为料液比1∶21(g/mL)、酶解时间71 min、超声时间21 min、纤维素酶添加量0.85%(以提取液质量为基准),多糖得率为
7.86%±0.13%。
抗氧化活性试验表明,羊肚菌多糖具有较好地清除DPPH·和·OH 的能力,抗氧化活性较好。
【总页数】6页(P128-133)
【作者】贾庆超
【作者单位】郑州科技学院食品科学与工程学院
【正文语种】中文
【中图分类】TS201.2
【相关文献】
1.超声波辅助提取羊肚菌菌丝体多糖的研究
2.尖顶羊肚菌多糖的超声波辅助提取工艺优化及其对肝损伤小鼠抗氧化活性的影响
3.羊肚菌多糖提取及其抗氧化活性研究
4.基于离子液体辅助提取的羊肚菌HPLC指纹图谱分析
5.碱性电解水提取对羊肚菌多糖性质及抗氧化活性的影响
因版权原因，仅展示原文概要，查看原文内容请购买。
水葫芦叶中总黄酮的提取及其抗氧化性研究
水葫芦叶中总黄酮的提取及其抗氧化性研究作者：许丽丽，蔡文军来源：《湖北农业科学》 2013年第5期许丽丽，蔡文军（韩山师范学院化学系，广东潮州５２１０４１）摘要：为研究水葫芦（Ｅｉｃｈｈｏｒｎｉａｃｒａｓｓｉｐｅｓ）叶中总黄酮的超声波法提取工艺，并测定其抗氧化活性，通过单因素试验和正交试验优化提取条件，对总黄酮还原能力及清除自由基能力进行测定。
结果表明，水葫芦叶中总黄酮最佳提取条件为超声功率３２０Ｗ、乙醇浓度７０％、超声时间３０ｍｉｎ、料液比１∶４５、提取次数３次，此条件下总黄酮得率为５．７１％，提取物呈现出良好的抗氧化活性。
关键词：水葫芦（Ｅｉｃｈｈｏｒｎｉａｃｒａｓｓｉｐｅｓ）叶；总黄酮；超声波；提取；抗氧化性中图分类号：Ｒ２８４．２文献标识码：Ａ文章编号：0439－８114（２０13）05－1131-03水葫芦（Ｅｉｃｈｈｏｒｎｉａｃｒａｓｓｉｐｅｓ）又名凤眼莲、洋水仙、水生风信子等，是雨久花科凤眼莲属的多年生漂浮水生草本植物［１］。
水葫芦繁殖速度快，生命力旺盛，而且往往缺乏天敌，所以在水域中常形成单一的优势群体，污染水体、破坏水中生态平衡，影响水产品的产量和质量，为蚊蝇孳生提供场所，阻碍水上交通。
多年来，水葫芦的防治问题一直是令很多国家的专家都头疼的问题，被公认为“世界十大害草”之一。
中国也深受水葫芦的危害，因此，许多科学家一直致力于研究水葫芦的物理、化学和生物防治方法。
另外，如何将这一害草变废为宝，以提高其资源利用率，也是近年来的研究热点［２，３］。
黄酮类化合物是广泛存在于植物界的一大类天然产物，具有抗氧化、抗衰老、抗辐射、抗肿瘤、抑菌抗病毒、抗心脑血管疾病、降血糖、调节免疫、治疗骨质疏松等作用［４，５］。
本试验利用的超声提取法具有能耗低、效率高、不破坏有效成分等优点，将超声技术应用于提取水葫芦叶中的黄酮类物质并测定提取物的抗氧化活性，可为水葫芦的综合利用提供科学依据。
１材料与方法１．１试验材料采集来自广东省潮州市卧石村的水葫芦叶，洗净，自然晾干后于６０℃烘干，粉碎并过６０目筛，再于６０℃烘干至恒重，得水葫芦叶干粉，置于干燥器中保存备用。
超声波辅助提取甘草总黄酮及其抗氧化性
超声波辅助提取甘草总黄酮及其抗氧化性
邹玉红;寇小燕;韩秋霞
【期刊名称】《食品研究与开发》
【年(卷),期】2011(032)009
【摘要】采用正交设计试验优化甘草总黄酮提取工艺,并研究其自由基清除活性.结果显示:超声波辅助提取甘草总黄酮的最佳提取工艺:乙醇浓度为75％、料液比为1:25、超声频率为350W,超声时间为25 min.总黄酮得率为1.943％；甘草总黄酮对自由基的清除能力随浓度的增大而增强,当溶液浓度达到1.1296 mg/mL时,甘草总黄酮对羟自由基(·OH)的清除率达到了55.73％,对超氧自由基(O2-·)的清除率达到50％.甘草总黄酮是一种天然有效的自由基清除剂,具有一定的抗氧化活性.【总页数】3页(P79-81)
【作者】邹玉红;寇小燕;韩秋霞
【作者单位】山东科技大学,山东青岛266510;山东科技大学,山东青岛266510;山东科技大学,山东青岛266510
【正文语种】中文
【相关文献】
1.超声波辅助提取葛根中总黄酮及其体外抗氧化性的研究 [J], 朱德艳;陈晗
2.超声波辅助提取羊奶果提取物中总黄酮及其抗氧化性研究 [J], 李扬; 邵永明
3.超声波辅助黄芩总黄酮提取及抗氧化性能研究 [J], 辛莹娟;李祯
4.超声波辅助双水相提取枇杷花总黄酮工艺优化及其抗氧化性 [J], 杨子敬;饶桂维;
王磊
5.藤三七总黄酮的超声波辅助提取及其抗氧化性研究 [J], 杨申明;王振吉;戴玥因版权原因，仅展示原文概要，查看原文内容请购买。
超声辅助提取首乌藤黄酮及其抗氧化活性的研究
超声辅助提取首乌藤黄酮及其抗氧化活性的研究肖扬;段玉峰【期刊名称】《农产品加工·学刊》【年(卷),期】2009(000)006【摘要】首乌藤是传统的药食同源植物,为进一步研究其生物活性成分,以乙醇溶液浸提,结合超声波辅助方法,采用L9(34)正交实验设计研究了首乌藤黄酮的最佳提取工艺,并测定了其对羟自由基(·OH)和1,1-二苯基-2-苦苯肼自由基(DPPH·)的清除结果.结果表明,黄酮最佳提取工艺条件为:提取温度60℃,乙醇体积分数50%,提取时间40 min,超声波功率200 W,料液比1:15,提取次数2次,该条件下总提取率可达21.35%.在一定范围内,提取物对·OH的清除效果与其浓度呈线性关系(R2=0.994 7),IC50为0.130 mg/mL;对DPPH·有较强的清除能力,其IC50值为0.032mg/mL.试验表明,首乌藤含有丰富的黄酮类化合物,具有体外抗氧化活性,是天然的自由基清除剂,有很大的开发前景.【总页数】4页(P38-41)【作者】肖扬;段玉峰【作者单位】陕西师范大学,食品工程与营养科学学院,陕西,西安,710062;陕西师范大学,食品工程与营养科学学院,陕西,西安,710062【正文语种】中文【中图分类】Q946-3【相关文献】1.黄花草总黄酮超声辅助提取工艺优化及抗氧化活性研究 [J], 许建本; 苏秀芳; 黄妹胶2.超声辅助提取款冬总黄酮工艺及抗氧化活性研究 [J], 陈苏丹; 汪亚祺; 李秀珍; 李学强3.超声辅助提取柚籽中黄酮及其抗氧化活性研究 [J], 李咏梅;谢婧4.响应曲面法优化超声辅助提取芒果叶中多酚和黄酮工艺及抗氧化活性研究 [J], 张静;陶俊葓;刘银;刘倩;杨周昊;李孟容;程桂广5.响应面法优化超声辅助提取肉豆蔻总黄酮工艺及其抗氧化活性研究 [J], 卓微伟;李凤;胡君因版权原因，仅展示原文概要，查看原文内容请购买。
超声波辅助亚临界水提取荜茇总黄酮工艺优化及其抗氧化活性评价
超声波辅助亚临界水提取荜茇总黄酮工艺优化及其抗氧化活性评价廖子蔚;胡辉;袁咏红;陈秀云;黄茜茜;龙林;孙代华【期刊名称】《中国食品添加剂》【年(卷),期】2024(35)2【摘要】采用超声波协同亚临界水技术进行荜茇中黄酮类成分的提取条件研究,并对其不同部位的总黄酮提取物进行抗氧化性对比分析。
结果表明,超声波协同亚临界水提取荜茇整株总黄酮最佳工艺条件为超声温度50℃,超声功率240 W,超声时间40 min,料液比1∶30(g/mL),亚临界水提取温度125℃,亚临界水提取时间为40 min,在此工艺条件下荜茇整株总黄酮最高提取量为(30±0.05)mg/g。
不同部位总黄酮提取物对DPPH自由基和超氧阴离子自由基清除能力的大小顺序为果穗>叶>根>茎,DPPH自由基清除率和超氧阴离子自由基清除率的IC50值分别为荜茇果穗37.96、304.33μg/mL,荜茇叶44.55、384.36μg/mL,荜茇根47.68、461.54μg/mL,荜茇茎130.60、487.80μg/mL。
采用超声波协同亚临界水提取荜茇整株总黄酮的工艺条件合理,提取得到的总黄酮具有良好的抗氧化性。
【总页数】11页(P32-42)【作者】廖子蔚;胡辉;袁咏红;陈秀云;黄茜茜;龙林;孙代华【作者单位】劲牌持正堂药业有限公司;湖北省中药配方颗粒工程技术研究中心【正文语种】中文【中图分类】TS202.1;TS201.1【相关文献】1.超声波辅助双水相体系优化橘红花总黄酮提取工艺及其抗氧化活性2.百香果皮总黄酮的复合酶辅助超声波提取工艺优化及其抗氧化活性分析3.表面活性剂辅助超声波提取橘红胎总黄酮工艺优化及其抗氧化活性4.红苋菜总黄酮超声波辅助提取工艺优化及其抗氧化、抑菌活性5.亚临界水提取苣荬菜总黄酮的工艺优化及其抗氧化活性研究因版权原因，仅展示原文概要，查看原文内容请购买。
赶黄草花、叶、杆中总黄酮含量及其抗氧化性比较研究
第52卷第12期 辽 宁 化 工 Vol.52，No.12 2023年12月 Liaoning Chemical Industry December，2023基金项目：四川省大学生创新创业训练项目（S202114389068）,烹饪科学四川省高等学校重点实验室（NO.PRKX201811）。
收稿日期： 2022-12-16赶黄草花、叶、杆中总黄酮含量及其抗氧化性比较研究陈诗琪，黄恬，蒲泠伶，王雪颖，叶峻*（成都师范学院 化学与生命科学学院，四川 成都 611130）摘 要：运用超声辅助-分光光度法优化了赶黄草花、叶、杆中总黄酮提取的料液比、超声时间、超声温度及超声功率等工艺条件及其含量测定。
结果表明：赶黄草花、叶、杆中总黄酮平均得率分别为：11.09%、9.27%、4.06%。
且样品的总黄酮提取液对DPPH ·、OH ·自由基均有良好的清除率，均超过66%。
结果表明：赶黄草花、叶、杆均有良好的抗氧化活性，具有明显的抗病毒、抗衰老等药效作用。
关 键 词：赶黄草；超声辅助；总黄酮；抗氧化活性中图分类号：X787 文献标识码： A 文章编号： 1004-0935（2023）12-1771-04赶黄草为虎耳草科扯根菜属多年生草本植物，其所含黄酮类生物活性成分，可通过清除自由基，提高体内活性酶水平，降低受肝损模型动物血清中转氨酶水平等，具有治疗黄疸、胆囊炎、肝损伤和传染性肝炎等药效作用[1-2]，并具有减肥、神经保护、抗癌等生物功能[3-5]。
同时，超声波具有强烈的振动、空化效应和搅拌作用，有利于提高提取效率，且方法简单、提取物纯度高，并可避免高温对提取成分的影响[6-8]。
本研究采用超声辅助提取法优化赶黄草花、叶、杆中黄酮类物质的提取工艺，并比较赶黄草的花、叶、杆黄酮类物质的含量及其对DPPH ·和OH ·自由基的清除率，为探究赶黄草的药效作用及综合开发提供参考。
橙叶总黄酮的超声波辅助提取工艺优化及性质探究
橙叶总黄酮的超声波辅助提取工艺优化及性质探究摘要：橙叶总黄酮（CWT）是一种天然含量丰富的有机化合物，具有重要的药理活性，但因为不易萃取等技术原因，导致在实际应用中存在犹豫不决的情况。
因此，本研究以橙叶总黄酮为目标物质，采用超声波辅助法进行提取，结合实验结果，优化提取参数，综合评价提取过程的性质，为其后续的开发利用提供理论依据。
关键词：橙叶总黄酮；超声波辅助提取；优化；性质探究１．言橙叶黄酮（CWT）是一种天然含量丰富的有机化合物，具有重要的药理活性。
它可以有效抑制心脏病、肝癌和血管病等疾病，是各种植物及其精油中的重要组成部分[1]，具有多种药理活性，如抗炎、抗肿瘤、抗衰老等作用。
但是，橙叶总黄酮的含量在植物中不高，利用普通的手段萃取困难，成本偏高，但因为其药理活性的重要性，提取它变得十分必要和重要。
目前，在橙叶总黄酮提取方面，有许多不同的方法，其中超声波辅助提取受到广泛关注[2]，它可以节省时间，降低能耗，减少有毒有害物质的污染。
因此，本研究拟采用超声波辅助法进行提取，结合实验结果，优化提取参数，综合评价提取过程的性质，为其后续的开发利用提供理论依据。
2.料与方法2.1料植物材料采自有礼貌植物园，将植物样品经搅碎处理，过筛（60μm），粉末用纱布筛分，得到固体样品，储存在实验室低温（-20℃）状态下，取用前放置室温发挥。
溶液中的原料称量于实验室常温下，加入超声波处理后，用滤筒过滤，得到提取物。
2.2声波辅助提取采用台式超声波振荡器，频率为20KHz，振荡器容积为1000 mL，超声功率为300W，提取温度为50℃，提取时间控制在30min内，提取时在3-5min内改变温度，提取时间控制在30min内，连续提取5次取平均值。
滤筛上选择直径为0.45μm的滤纸，滤出的提取物称量，以计算橙叶总黄酮的提取率。
3.果与讨论3.1取过程中不同参数的影响以上述参数为基础，用实验来研究不同参数在超声波辅助提取过程中的影响，用实验结果来优化变量，如振荡器容积、提取温度、提取时间等，以达到最佳提取率，再结合实际生产情况，将用于实际生产的参数优化确定下来，以供参考。
超声波辅助提取田基黄多酚类和黄酮类化合物及其抗氧化活性研究
超声波辅助提取田基黄多酚类和黄酮类化合物及其抗氧化活性研究汤须崇;蔡婀娜【摘要】采用超声技术从田基黄中提取活性物质.运用响应面法确定超声提取田基黄的最佳条件.运用单因素试验选取三个自变量.采用Box-Behnken设计评价这三个自变量对总黄酮和总多酚提取、DPPH和ABTS+活性清除的影响.通过方差分析显示,二次模型对反应的贡献率具有统计学意义.运用响应面法进行最优化研究,并用数学模型绘制出三维响应面.通过结合反应得出最佳试验条件:超声时间48.89 min,乙醇浓度63.72％,超声温度66.92℃.总黄酮值为105.06 mg RE/g DW,总多酚值为51.75 mg GAE/g DW,％DPPHsc为58.81％,％ABTSsc为64.99％.在最佳试验条件下,试验值与方差分析预测值一致.结果表明,采用四个模型和响应面法优化总黄酮和总多酚的提取、DPPH和ABTS+活性清除是切实可行的.【期刊名称】《天然产物研究与开发》【年(卷),期】2014(026)005【总页数】12页(P750-760,805)【关键词】田基黄;总黄酮;总多酚;DPPH;ABTS;响应面法【作者】汤须崇;蔡婀娜【作者单位】华侨大学化工学院,厦门361021;华侨大学化工学院,厦门361021【正文语种】中文【中图分类】R284.1IntroductionHypericum japonicum，locally called‘Tian-ji-huang’，is prepared from the entire herb of H.japonicum Thunb.ex Murray (Hypericaceae).It is one of traditional Chinese medicines (TCM)widely distributed in the south of the Yangtze River，China［1］.H.japonicum has been used for the treatment of bacterial diseases，infectious hepatitis，gastrointestinal disorder，internal hemorrhage and tumors［2-6］.As reported previously，H.japonicum mainly contains xanthones［6，7］，chromenes［8］，flavonoids［9，10］，dipeptide derivatives［11］，polyphenols and phloroglucinol derivatives［12］.Some of these constituents are known to exhibit pharmacological and biological activities［13］.It has long been recognized that polyphenol and flavonoid are an important class of antioxidants［14］.Antioxidants play an indispensable role as health benefactors in human life and are also added to food to prevent or delay its oxidation［15］.Synthetic antioxidants are widely used since they are more effective and cheaper than natural ones.However，the safety and toxicity of synthetic antioxidants have brought great concerns.Thus，it is essential to develop and utilize effective and natural antioxidant to protect the body［16］.In the present study，the total phenol content (TPC)and total flavonoid content (TFC)of H.japonicum were chosen to determine their antioxidant activities.Recently，ultrasonic extraction method has been widely employed to extract bioactive components from plant material due to its highextraction efficiency［17］.Response surface methodology (RSM)is a relatively new method for optimizing experimental conditions.In the present study，the ultrasonic technique was employed to extract bioactive components from H.japonicum.Response surface methodology and Box-Behnken design were used to evaluate the effects of ultrasonic time，temperature and ethanol concentration，which were chosen according to the single factor study，on the extraction of bioactive components and free radical scavenging activity (determined by DPPH and ABTS+ methods)of H.japonicum.Materials and InstrumentsMaterials and chemicalsHypericum japonicum was purchased from a drug store in Fujian Province of China and stored at 4 ℃till tested.Folin-ciocalteu reagent，1，1-Diphenyl-2-picrylhydrazyl (DPPH)，2，2’-azinobis-3-ethylbenzothiazoline -6-sulfonic acid (ABTS)，butylated hydroxytoluene(BHT)，6-hydroxy-2，5，7，8-tetramethylchroman-2-carboxylic acid (Trolox)were purchased from Sigma company.Deionized water was used throughout the experiment.All other chemicals used were of analytical grade.InstrumentsUV-Visible spectra were measured using Spectra(Pharmaspec UV-2550，Shimadzu，Kyoto，Japan)spectrophotometer.The ultrasonic assisted extraction was carried out in a KQ-600E ultrasonic device (Changzhou Nuoji Instrument Company，China)with an ultrasonic power of 600 W，heating power of 800 W and frequency of 40 kHz，equipped with a digitaltime and a temperature controller.MethodsSample preparationH.japonicum was d ried at 60 ℃till constant weight.The dried material was pulverized to 100 meshes.The powdered H.japonicum was accurately weighted and then ultrasonically extracted once with ethanol (40 mL)for special time.The supernatant solution was combined，filtrated and then cooled down to room temperature.The solution was transferred to a 100 mL volumetric flask and topped up to the volume with ethanol.Single factor experiments for TFC extractionThe effects of five experimental variables on extraction yield of TFC were investigated by single factor tests.Five experimental variables were liquid-to-solid ratio(10，15，20，25，30)，ultrasonic time (20，30，40，50，60 min)，power (50%，60%，70%，80%，90%，100%)，temperature (30，40，50，60，70 ℃)and ethanol concentration (50%，60%，70%，80%，90%).Determination of TFC contentThe TFC was determined by the modified aluminum chloride colorimetric method［18］with rutin as standard.Each of the plant extracts (2 mL，1.6 mg/mL)or rutin (0.222 mg/mL)was added to 30% ethanol concentration (4 mL)and 5% NaNO2solution (1 mL).After 6 min，10% Al(NO3)3solution (1 mL)was added.After another 6 min，4% NaOH solution (10 mL)was added，and the volume was made up with 30%ethanol.The mixture was shaken thoroughly and measured at 510 nm.The results were expressed asmilligram Rutin equivalents/g of dry plant material.The calibration curve of rutin was y=12.671x-0.0125，R2=0.9998 (0.00888-0.05328 mg/mL).Here，y=absorbance and x=concentration.All experiments were done in triplicate.Determination of TPC contentThe TPC was determined by the modified Folin-Ciocalteu method［19］with gallic acid as standard.Each of the plant extracts (1 mL，1.6 mg/mL)or gallic acid (150 μg/mL)was added to deionized water (10 mL)and Folin-Ciocalteu reagent (1.5 mL).After 30s，10%Na2CO3(6 mL)was added to the mixture.The mixture was shaken thoroughly and allowed to stand at30 ℃for 2 h in the dark.The absorbance was measured at 765 nm.The results were expressed in mg Gallic acid equivalent/g of dry plant material. The calibration curve of gallic acid was y=129.34x-0.0125，R2=0.9993 (0.000616-0.00616 mg/mL).Here，y=absorbance and x=concentration.All experiments were done in triplicate.DPPH and ABTS+ free radical scavenging activity assayDPPH assayThe DPPH free radical scavenging activity of the extracts was determined using the reported method［20］.Equal volumes (800 μL)of different concentrations of the extracts and ethanol (1200 μL)were added with0.1mM DPPH (2000 μL).The mixture was measured at 517 nm after 30 min of incubation at 37 ℃in the dark.The %DP PHsc was determined using the following formula:%DPPHsc=［1-(As-A0)/Ac］×100As:sample (800 μL)+ethanol (1200 μL)+0.1mM DPPH (2000 μL)A0:sample (800 μL)+ethanol (3200 μL)Ac:ethanol (2000 μL)+0.1 mM DPPH (2000 μL)The IC50was calculated from the graph of scavenging effect percentage against extract concentration.Synthetic antioxidants (Trolox and BHT)were used as control，and all tests were performed in triplicate.ABTS+· assayABTS+ free radical was produced by reacting 2，2’-azinobis ［3-ethylbenzothiazoline-6-sulphonic acid］(ABTS)with potassium persulfate (K2S2O8).ABTSassay was carried out，according to the reported method ［21］with slight modification.ABTS solution (2000 μL)was added to eachof the samples (800 μL)，and mixed vigorously.The reaction mixture was kept at room temperature for 7 min before the absorbance was measured at 734 nm.The %ABTSsc was determined using the followingformula:%ABTSsc=［1-(As-A0)/Ac］×100As:sample (800 μL)+ethanol (1200 μL)+ABTS(2000 μL)A0:sample (800 μL)+ethanol (3200 μL)Ac:etha nol (2000 μL)+ABTS(2000 μL)The IC50was calculated from the graph of scavenging effect percentage against extract concentration.Synthetic antioxidants (Trolox and BHT)were used as control，and all tests were performed in triplicate.Experimental designThe extraction parameters were optimized using response surface methodology (RSM).A Box-Behnken design (BBD)was employed for experimental design，data analysis and model building.Three variablesused in the study were ultrasonic time (X1)，ethanol concentration (X2)and temperature (X3).The symbols and levels presenting in Table 1 were based on single factor pre-test.TFC，TPC，%DPPHsc，%ABTSsc were selected as the responses for the combination of the independent variables given in Table 2.Three triplicate experiments were carried out at each experimental design point and the mean values were stated as observed responses.Experimental runs were randomized，to minimize the effects of unexpected variability in the observed responses.The variables were coded according to the following equation:X=(Xi-Xo)/△XWhere X is the coded value，Xi is the corresponding actual value，Xo is the actual value in the center of the domain，and △X is the increment of Xi corresponding to a variation of 1unit of X.The mathematical model corresponding to the Box-Behnken designis:Y=β0+β1X1+β2X2+β3X3+β11X12+β22X22+β33X32+β12X1X2+β13X1X3 +β23X2X3+εWhere Y is the dependent variable (TFC，TPC，%DPPHsc，%ABTSsc)，β is the model constant，βi，βii and βij are the model coefficients，and ε is the error.They represent the linear，quadratic and interaction effects of the variables.Analysis of the experimental design data and calculation of predicted responses were carried out using Design Expert software (version7.0，stat-Ease，Inc.，Minneapolis，MN).Additional confirmation experiments were subsequently conducted to verify the validity of the statistical experimental design.Table 1 Three factors and three levels design of RSM experimentResults and DiscussionSingle factor experiments for TFC extractionEffect of liquid-to-solid ratio on the extraction yield of TFCIn order to evaluate the effect of liquid-to-solid ratio on the extractionyield of TFC，different liquid-to-solid ratios (10，15，20，25 and 30)were tested.Other experimental parameters were set as follows:70% ethanol concentration;60 ℃ultrasonic temperature;100% ultrasonic power;30 min ultrasonic time.The results were shown in Fig.1.Fig.1 Effect of liquid-to-solid ratio on the extraction yield of TFCThe extraction yield of TFC increased from 35.14 mg RE/g DW to 110.06mg RE/g DW as the liquid-tosolid ratio increased within the range of 10～25 (V/W).When the liquid-to-solid ratio increased to 30 (V/W)，the yield of TFC increased to 88.64 mg RE/g DW.The results indicated that 1∶25 was more suitable for the extraction of TFC.Effect of ethanol concentration on the extraction yield of TFCEthanol concentration was the most important step towards parameter optimization，which had a strong impact on extraction yield ofTFC.Different ethanol concentrations (50%，60%，70%，80% and90%)were tested in the experiment.Other experimental parameters wereset as follows∶1∶20 liquid-to-solid ratio;60 ℃ultrasonic temperature;100% ultrasonic power;30min ultrasonic time.The results were shown in Fig.2. Fig.2 Effect of ethanol concentration on the extraction yield of TFCThe extraction yield of TFC increased from 85.09 mg RE/g DW to 87.55 mg RE/g DW as the ethanol concentration increased from 50% to 60%.Whenthe ethanol concentration continued to increase up to 90%，the yield of TFC decreased to 61.90 mg RE/g DW.The results indicated that 60% ethanol concentration was suitable for the extraction of TFC.Effect of ultrasonic power on the extraction yield of TFCThe yield from the TFC extraction could be influenced by the ultrasonic power.Different ultrasonic powers(100%，90%，80%，70%，60% and 50%)were tested in the experiment.Other experimental parameters wereset as follows∶1∶25 liquid-to-solid ratio;70% ethanol concentration;60 ℃ ultrasonic temperature;30 min ultrasonic time.The results were shown in Fig.3.Fig.3 Effect of ultrasonic power on the extraction yield of TFCThe extraction yield of TFC changed within the range of 85.87 mg RE/g DW to 91.22 mg RE/g DW as the ultrasonic power increased from 50% to 100%.The ultrasonic power had little impact on the extraction yield of TFC. Effect of ultrasonic temperature on the extraction yield of TFCUltrasonic temperature was a factor that would significantly influence the extraction efficiency of TFC.Different ultrasonic temperatures (30，40，50，60 and 70 ℃)were tested in the experiment.Other experimental parameters were set as follows∶1∶25 liquid-to-solid ratio;60%ethanol concentration;100%ultrasonic power;30min ultrasonic time.The results were shown in Fig.4.Fig.4 Effect of ultrasonic temperature on the extraction yield of TFCThe extraction yield of TFC increased from 86.63 mg RE/g DW to 97.11mg RE/g DW as ultrasonic temperature increased from 30 ℃to 70 ℃.Itindicated ultrasonic temperature had a significant impact on the extraction yield of TFC.The resul ts showed that 70 ℃was suitable for the extraction of TFC.Effect of ultrasonic time on the extraction yield of TFCDifferent ultrasonic time (20，30，40，50，60 min)was tested in the experiment.Other experimental parameters were set as follows∶1∶25 liquid-to-solid ratio;60% ethanol concentration;100%ultrasonicpower;60 ℃ultrasonic temperature.The results were shown in Fig.5.Fig.5 Effect of ultrasonic time on the extraction yield of TFCThe extraction yield of TFC significantly increased from 97.73 mg RE/g DW to 102.66 mg RE/g DW as ultrasonic time increased from 20 min to 50 min.However，as ultrasonic time increased up to 60 min，the yield of TFC decreased to 94.64 mg RE/g DW.The result showed that 50 min was suitable for the extraction of TFC.Optimization of bioactive components and antioxidant activities by Response Surface Methodology(RSM)Three variables［ultrasonic time (X1)，ethanol concentration (X2)and temperature(X3)］，which had higher impact on the extraction yield of TFC，were selected according to single factor tests.The four responses variables were TFC，TPC，% DPPHsc，% ABTSsc.The results of 15 runs using BBD design were shown in Table 2.Table 2 BBD with observed responses for TFC，TPC，%DPPHscand %ABTSscaMean of triplicate determinations.Table 3 ANOVA for response surface quadratic model:estimated regression model of relationship between response variables and independent variables (X1，X2and X3)a.The coefficient of determination (R2)of the model was 0.9723.b.The coefficient of determination (R2)of the model was 0.9358.c.The coefficient of determination (R2)of the model was 0.9812.d.The coefficient of determination (R2)of the model was 0.9767.Model fittingTable 3 showed the results of fitting quadratic models to the data.The results of analysis of variance (ANOVA)indicated that the contribution of the quadratic model was significant.The significance of each coefficient was determined using the F-test and P-value in Table 3.The lack of fit was also used to verify the adequacy of the model.ANOVA for the lack of fit was not significant (P ＞0.05)for the model，indicating that the model can adequately fit the experiment data.Coefficient (R2)of determination was defined as the ratio of the explained variation to the total variation and was a measurement of the degree of fitness.The small value of R2indicated the poor relevance of the dependent variables in the model.The model can fit well with the actual data approaches unity.The mathematical models representing TFC，TPC，%DPPHsc，%ABTSsc as a function of the response variables within the region under investigation were expressed by the following equation:TFCIt can be seen that the variable with the largest effect on TFC extraction was the quadratic term of )followed by the linear terms of ultrasonic temperature(X3)and the quadratic terms of ultrasonic temperature)and ultrasonic time ()(P ＜0.01)，the linear term of ethanol concentration(X2)and the quadratic term of )were not significant，indicating that the relationship between response variable (TFC)and the process variables was not simply a linear one.The Model F-value of 19.50 implied the model was significant.The "Lack of Fit F-value" of 0.64 implied that the Lack of Fit was not significantly relative to the pure error.Non-significant lack of fit was good.R2 value of the model for TFC was determined to be 0.9723.These values gave a relative good fit to the mathematic model in Fig.6(A-C). TPCIt can be seen the variable with the largest effect on TPC extraction was the linear terms of ultrasonic temperature(X3)(P ＜0.01)and ethanol concentration(X2)followed by the quadratic term of ultrasonic time()，the linear of (X1)(P ＜0.05)，while the interaction terms were not significant (P ＞0.05)，indicating that the change of X1，X2，X3， had significant effects on TPC extraction.The Model F-value of 8.09 implied the model was significant.The "Lack of Fit Fvalue" of 0.18 implied the Lack of Fit was not significant relative to the pure error. Non-significant lack of fit was good.R2 value of the model for TFC was determined to be 0.9358.These values would give a relative good fit to the mathematic model in Fig.6(DF). %DPPHscIt can be seen the variable with the largest effect on DPPH scavengingactivity was the linear terms of ultrasonic temperature (X3)and the quadratic term of ultrasonic time ()，the interaction (X2X3)(P ＜0.01)，and (X1X3)，the linear term of (X1).It indicated that the relationship between response variable(%DPPHsc)and the process variables was not simply a linear one.The Model F-value of 29.01 implied the model was significant.The " Lack of Fit F-value" of 2.08 implied the Lack of Fit was not significant relative to the pure error.Non-significant lack of fit was good.R2 value of the model for %DPPHsc was determined to be 0.9812.These values gave a relative good fit to the mathematic model in Fig.6(G-I).%ABTSscIt can be seen the variable with the largest effect on ABTS scavenging activity was the linear terms of (X3)and (X2)followed by the quadratic terms of ultrasonic temperature ()and ethanol concentration()(P＜0.01)，the interaction (X1，X2)and (X1，X3)(P＜0.05)，indicating that the relationship between response variable (%ABTSsc)and the process variables was not simply a linear one.The Model F-value of 23.29 implied the model was significant.The "Lack of Fit F-value" of 0.79 impliesd the Lack of Fit was not significant relative to the pure error.Non-significant lack of fit was good .R2 value of the model for %ABTSsc was determined to be 0.9767.These values gave a relative good fit to the mathematic model in Fig.6(J-L).Interpretation of response surface methodGraphs of RSM directly reflected the impact of factors on the response value，which the extraction yield was corresponding to the factor X1，X2，X3consisting of a Three-dimensional response surface plot and two-dimensional contour plot.Its interactions during the procedure can be found from the response surface plot.The contour plot and response surface graph of TFC，TPC，% DPPHsc，%ABTSsc were shown in Fig.6. Fig.6 Response surface plots for extraction yield of TFC (A-C)，extraction yield of TPC (D-F)，%DPPH (G-I)and %ABTS (J-L)Optimization ultrasonic conditon by RSMTable 4 showed the optimal conditions for each individual response with the predicted and experimental values.Optimal conditions for TFC were:ultrasonic time of 50.58 min，ethanol concentration of 65.83% and ultrasonic temperature of 59.96 ℃.Optimal conditions for TPC were ultrasonic time of 49.59 min，ethanol concentration of 60.15% and ultrasonic temperature of 70.00 ℃.Optimal condition for %DPPHsc was ultrasonic time of 47.84 min，ethanol concentration of 80.00% and ultrasonic temperature of 70.00 ℃.Optimal condition for % ABTSsc was ultrasonic time of 41.78 min，ethanol concentration of 60.00% and ultrasonic temperature of 70.00 ℃.The conditions gaveTable 4 Predicted and experimental values under optimal conditions based on individual response (TFC，TPC，%DPPHsc，%ABTSsc)a:Analysis results were mean value.TFC，TPC，%DPPHsc and %ABTSsc values of 107.42 mg RE/g DW，51.98 mg GAE/g DW，63.06% and 66.40%，respectively.Table 5 showed that the three optimal conditions were based on combination of all responses.The optimal condition was ultrasonic time of48.89 min，ethanol concentration of 63.72% and ultrasonic temperature of 66.92 ℃.The condition gave TFC，TPC，% DPPHsc and %ABTSsc values of 105.06 mg RE/g DW，51.75 mg GAE/g DW，58.81% and 64.99%.Table 5 Predicted and experimental values under optimal conditions based on combination of responses (TFC，TPC，%DPPHscand %ABTSsc)a:Analysis results were mean values.Antioxidant activityThe extract of H.japonicum was chosen for the DPPH and ABTS scavenging assay，Trolox and BHT were used as positive control.The results were shown in Fig.7 and Fig.8.The IC50values of H.japonicum，BHT and Trolox in DPPH scavenging assays were 34.07 μg/mL，22.79 μg/mL and 2.78μg/mL，respectively.The IC50values of H.japonicum，BHT and Trolox in ABTSscavenging assays were 25.48 μg/mL，6.59 μg/mL and 1.39μg/mL.The results showed that the DPPH and ABTS free radical scavenging activities of H.japonicum were lower than the positive control(BHT and Trolox).Fig.7 DPPH free radical scavenging activity of H.japonicum，BHT and TroloxConclusionThe response surface methodology and Box-Behnken design were applied to evaluate the effects of three independent variables (ultrasonic time，ethanol concentration，ultrasonic temperature)on the extraction of TFC，TPC and the scavenging activities to DPPH and ABTS+ free radicals.The analysis of variance (ANOVA)indicated that the relationship betweenresponse variable (TFC，TPC，% DPPHsc，% ABTSsc)and the process variables was not simply linear one.Fig.8 ABTS + free radical scavenging activity of H.japonicum，BHT and TroloxFrom the data of the 3D response plots and model equations of TFC，TPC，%DPPHsc，%ABTSsc，the optimal conditions of each individual response and all responses were determined to be:The optimal conditions of each individual response:Optimal conditions for TFC were:ultrasonic time of 50.58 min，ethanol concentration of 65.83% and ultrasonic temperature of 59.96 ℃.Optimal condition s for TPC were ultrasonic time of 49.59 min，ethanol concentration of 60.15% and ultrasonic temperature of 70.00℃.Optimal conditions for % DPPHsc were ultrasonic time of 47.84 min，ethanol concentration of 80.00%and ultrasonic temperature of 70.00 ℃.Optimal conditions for %ABTSsc were ultrasonic time of 41.78 min，ethanol concentration of 60.00% and ultrasonic temperature of 70.00 ℃.Under these optimized conditions，The yields of TFC and TPC were 107.42 mg RE/g DW and 51.98 mg GAE/g DW.The %DPPHsc and%ABTSsc values were 63.06% and 66.40%.The optimal conditions of all responses:ultrasonic time of 48.89 min，ethanol concentration of 63.72% and ultrasonic temperature of66.92 ℃.The optimal conditions gave TFC，TPC，%DPPHsc and %ABTSsc values of 105.06 mg RE/g DW，51.75 mg GAE/g DW，58.81% and 64.99%，respectively.Under these optical conditions，the experimental values agreed with 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橙叶总黄酮的超声波辅助提取工艺优化及性质探究
橙叶总黄酮的超声波辅助提取工艺优化及性质探究
李丹;汪秀妹;何雅婷
【期刊名称】《莆田学院学报》
【年(卷),期】2022(29)2
【摘要】为开发和利用橙叶总黄酮资源,采用单因素试验结合响应面分析法对超声辅助提取橙叶总黄酮的工艺参数进行优化。
研究了橙叶总黄酮粗提液体外抗氧化活性和对大肠杆菌的抑制作用。
结果表明,最佳提取工艺为:乙醇浓度58%、料液比1∶42 g/mL、超声浸提温度71℃、超声浸提时间30 min、超声功率420 W,总黄酮得率为(7.64±0.03)%。
橙叶总黄酮对ABTS;·的半抑制浓度为20.95 mg/L,对Fe;的还原能力随样品浓度的增大而增大,对大肠杆菌的最低抑制浓度为12.5 g/L。
【总页数】7页(P50-55)
【作者】李丹;汪秀妹;何雅婷
【作者单位】莆田学院环境与生物工程学院;福建省新型污染物生态毒理效应与控制重点实验室;生态环境及其信息图谱福建省高等学校重点实验室
【正文语种】中文
【中图分类】R318
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