CN113041278A - 一种提取油菜苔结合态多酚的方法 - Google Patents
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Abstract
本发明涉及一种从油菜苔中提取结合态多酚的工艺技术，其步骤为油菜苔粉末经80％丙酮超声，过滤后所得滤渣进行冻干，之后用2mol/L NaOH溶液进行水浴，然后用6mol/L的盐酸将溶液pH值调至2，过滤后的滤液使用乙酸乙酯进行萃取，萃取液经浓缩后冷冻干燥得到油菜苔结合态多酚。该工艺大大地提高了结合态多酚得率和纯度，整个分离过程对环境要求不高，纯度最高，分离材料便宜易得，分离操作过程简单，人工易控制，且纯化效率高。
Description
所属技术领域
本发明涉及一种提取油菜苔中结合态多酚的工艺，属于植物提取技术领域。
背景技术
油菜苔为十字花科植物，油菜的嫩茎叶，别名芸苔、寒菜、胡菜、苦菜、苔芥,性凉，味甘，入肝、脾、肺经，具有活血化瘀，解毒消肿，宽肠通便，强身健体等功效。油菜苔的食疗作用在于降低血脂，解毒消肿，宽肠通便，强身健体等。
结合态多酚主要是指结合于细胞壁上的一些水合单宁酸和原花青素，通常通过化学或者酶处理方法，打破多酚物质与细胞壁结合的化学键，才将其分离出来的部分。结合态多酚具有各种生物活性；抗氧化潜力、抗炎活性强，在抑制结肠癌细胞生长和集落形成方面十分有效；同时还具有有效诱导人结肠癌细胞的细胞周期停滞和细胞凋亡的活性。
公开号为CN104189582A的中国专利公开了一种谷糠内壳结合态多酚及其制备方法,以及该多酚在制备抗肿瘤药物和保健食品中的应用。其制备方法是将纯天然谷糠内壳粉碎后,称取适量,用预冷 80％丙酮充分搅拌混匀后将混合物离心,收集残留固体物质用2mol/L NaOH消化；消化一定时间后用浓盐酸滴定终止消化,使溶液pH为7；随后加入正己烷和乙酸乙酯萃取数次除去脂质；离心收集上清；将上述提取液旋转蒸发至一定体积,再真空冷冻干燥成粉末,即得到谷糠内壳结合态多酚。体外抗肿瘤实验表明，该结合态多酚具有广谱性抗肿瘤活性,为开发研制新型抗癌保健品或药物提供了可能。
公开号为CN111514174A的中国专利公开了一种沙棘果结合态多酚的提取方法,包括以下步骤；1) 取新鲜的沙棘果适量,清洗干净后榨汁制成沙棘果汁备用；2)按照沙棘果和乙醇的重量体积比为1g： 10～15mL的量量取乙醇溶液,-18～-22℃下预冷,然后将乙醇溶液加入步骤1)中制好的沙棘果汁中, 搅拌均匀后离心,弃上清液,收集残渣,重复进行1～2次；3)将步骤2)中收集的残渣中加入2M的NaOH 碱水解液,在室温下充分搅拌至残渣完全消化,然后加入适量的浓盐酸溶液调节溶液的pH至中性；4) 将步骤3)中制备的溶液离心,离心后取上清液弃沉淀,然后在上清液中加入等体积的乙酸乙酯萃取, 且重复萃取4-5次后离心取下层水相,即得到结合态多酚提取液；5)将步骤4)中得到的结合态多酚提取液在45-50℃下旋转蒸发,除去残留有机溶剂,然后在真空冷冻干燥水溶液至形成粉末,即得到结合态多酚样品。
公开号为CN109222096A的中国专利公开了一种胡萝卜膳食纤维中结合多酚的提取方法，包括以下步骤；(1)取胡萝卜副产品烘干粉碎得到胡萝卜粉,将胡萝卜粉以料液质量比1∶8.5与去离子水混合,之后依次加入耐高温α-淀粉酶、木瓜蛋白酶和糖化酶分别水解30min以去除淀粉和蛋白质；将水解的混合物经90％的乙醇和丙酮洗涤之后真空干燥得到胡萝卜膳食纤维。(2)将步骤(1)得到的胡萝卜膳食纤维加入棕色螺旋管中用氢氧化钠溶液处理,同时冲入氮气以隔绝空气反应4h,之后用盐酸调节溶液pH至1.5-2之间并放置10min；然后加入两倍体积的乙醇溶液萃取30min,过滤,如此反复操作 2-4次,合并每次操作所得的滤液；将滤液真空浓缩后冷冻干燥得到结合多酚。
结合态多酚在油菜苔中有一定含量，且原料简单易得，分布广泛，价格便宜。目前国内外公开的文献资料尚未有对其进行综合研究和开发利用的，因而对油菜苔中结合态多酚的提取研究有一定的意义。
发明内容
本发明采用的技术方案包括：冻干过后的油菜苔粉末经丙酮超声、冻干、用碱溶液水浴提取、调节pH、乙酸乙酯萃取、浓缩、冻干制得结合态多酚粗提物。
因此，本发明提供一种制备结合态多酚粗提物的方法，步骤包括：
(1)取油菜苔冻干粉在丙酮浓度为80％，液料比30mL/g，提取时间30min，超声功率为210w的条件下，重复提取三次，抽滤分离得上清液A和残渣A；
(2)将滤渣A用甲醇洗3次，蒸馏水洗3次，冻干后再用粉碎机打成细粉过40目筛；
(3)将滤渣A粉末用2mol/L NaOH溶液以1:20(g/mL)的料液比在100℃下水浴加热4.5h；
(4)用6mol/L的盐酸将水解液pH值调到2，抽滤分离得到上清液B和残渣B；
(5)使用等体积的乙酸乙酯(体积比1:1)萃取上清液B，重复萃取三次，合并萃取液后在40℃旋转蒸发，最后将浓缩物冷冻干燥，即得到结合态多酚(NEP)。
技术效果
1、通过丙酮去除游离多酚，加碱水浴处理油菜苔渣粉，提取油菜苔结合态多酚，分离操作过程简单，人工易控制，且纯化效率高。
2、该法大大地提高了结合态多酚得率和纯度，整个分离过程对环境要求不高，纯度最高，分离材料便宜易得。
具休实施方式
下面，本发明将用实施例进行进一步的说明，但是它并不限于这些实施例的任何一个或类似实例。
实施例1
取100g油菜苔冻干、粉碎至40目以下，在丙酮浓度为80％，液料比30mL/g，提取时间30min，超声功率为210w的条件下，重复提取三次，抽滤分离得残渣；将滤渣用甲醇洗3次，蒸馏水洗3次，冻干后再用粉碎机打成细粉过40目筛。将滤渣冻干粉用4mol/L NaOH溶液以1:20(g/mL)的料液比在85℃下水浴加热10h，再用6mol/L的盐酸将水解液pH值调到2，抽滤分离得到上清液。使用等体积的乙酸乙酯(体积比1:1)萃取上清液，重复萃取三次，合并萃取液后在40℃旋转蒸发，最后将浓缩物冷冻干燥，即得到结合态多酚，提取率为1.834mg/g。
实施例2
取100g油菜苔冻干、粉碎至40目以下，在丙酮浓度为80％，液料比30mL/g，提取时间30min，超声功率为210w的条件下，重复提取三次，抽滤分离得残渣；将滤渣用甲醇洗3次，蒸馏水洗3次，冻干后再用粉碎机打成细粉过40目筛。将滤渣冻干粉用2mol/L NaOH溶液以1:20(g/mL)的料液比在95℃下水浴加热10h，再用6mol/L的盐酸将水解液pH值调到2，抽滤分离得到上清液。使用等体积的乙酸乙酯(体积比1:1)萃取上清液，重复萃取三次，合并萃取液后在40℃旋转蒸发，最后将浓缩物冷冻干燥，即得到结合态多酚，提取率为2.186mg/g。
Claims (1)
1.一种制备油菜苔结合多酚的方法，步骤包括：
(1)取油菜苔冻干粉在丙酮浓度为80％，液料比30mL/g，提取时间30min，超声功率为210w的条件下，重复提取三次，抽滤分离得上清液A和残渣A；
(2)将滤渣A用甲醇洗3次，蒸馏水洗3次，冻干后再用粉碎机打成细粉过40目筛；
(3)将滤渣A粉末用2mol/LNaOH溶液以1:20(g/mL)的料液比在100℃下水浴加热4.5h；
(4)用6mol/L的盐酸将水解液pH值调到2，抽滤分离得到上清液B和残渣B；
(5)使用等体积的乙酸乙酯(体积比1:1)萃取上清液B，重复萃取三次，合并萃取液后在40℃旋转蒸发，最后将浓缩物冷冻干燥，即得到油菜苔结合多酚。
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| CN114451534A (zh) * | 2022-01-28 | 2022-05-10 | 湖南农业大学 | 低盐短时发酵预处理与干燥气蒸相结合干制油菜苔的加工方法 |
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| CN113730951A (zh) * | 2021-08-02 | 2021-12-03 | 江苏大学 | 提高高粱麸皮结合态多酚抗氧化活性的亚临界水萃取方法 |
| CN114451534A (zh) * | 2022-01-28 | 2022-05-10 | 湖南农业大学 | 低盐短时发酵预处理与干燥气蒸相结合干制油菜苔的加工方法 |
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