CN107737036A - 一种以 1,3‑丁二醇为溶剂从油茶茶籽皮中提取抗氧化成分的方法 - Google Patents
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Abstract
本发明公开了一种以1,3‑丁二醇为溶剂从油茶茶籽皮中提取抗氧化成分的方法。1,3‑丁二醇在化妆品中常做为保湿剂，以1,3‑丁二醇直接作为溶剂从油茶茶籽皮中提取抗氧化成分用于面膜等化妆品的制造具有许多显著优点。该发明的技术要点是：首先将茶籽皮进行粉碎过筛后，先以正己烷萃取，除去茶籽皮中油脂类物质；接着用丁二醇为溶剂，进行搅拌提取，提取液，蝶式离心分离，除去大颗粒沉淀，接着通过陶瓷膜分离设备，除去大分子蛋白及多糖类物质，滤出液为茶籽皮有效成分，可直接用于化妆品、护肤品的添加。该方法提取物抗氧化能力强，抗氧化物纯度高，能耗低，产品不受微生物污染。
Description
技术领域
本发明属于天然产物领域，涵盖农林资源综合利用，可直接用于化妆品、护肤品的添加，应用于美容美妆行业。具体涉及一种以1,3-丁二醇(保湿剂)为溶剂从油茶种皮中提取制备抗氧化成分的方法。
背景技术
油茶(Camellia oleifera Abel.)山茶科山茶属，是我国特有的木本油料树种；广泛种植于我国亚热带丘陵地区，与乌桕、油桐和核桃并称为我国四大木本油料植物。油茶具有种植成活率高，不与粮棉争地的优势，在经济、社会、生态等各方面效益显著，对维护国家粮油安全、发展南方山区经济、改善国民食用油结构等均具有重大意义，受到国家的高度重视，发展前景广阔。
现阶段，对油茶资源的利用主要集中在茶籽榨取食用油上，茶油富含不饱和脂肪酸，是媲美橄榄油的优质油料，在医疗保健上也有一定疗效。对于榨油余料如茶籽皮、茶枯饼的利用程度相对较低，一般将其作为动植物饲料和食用菌的培养基，或用于茶皂素及活性炭等化工原料的提取。现代药理学研究表明，茶籽皮中富含黄酮类，茶皂素，萜类等酚类物质，这些化合物具有很强的抗氧化及抗炎抗菌活性。到目前为止，这些化合物的提取都是以水、乙醇、甲醇做溶剂，然后再综合采用其他分离技术，干燥制备提取物成品，这样导致了高能耗且造成了抗氧化性能的破坏。
发明内容
本发明旨在克服现有技术的不足，提供一种能直接应用于化妆品的以保湿剂1,3-丁二醇为溶剂从油茶种皮中提取制备抗氧化成分的方法，为油茶资源的全方位综合利用提供新方向。
为了达到上述目的，本发明提供的技术方案为：
所述以1,3-丁二醇为溶剂从油茶种皮中提取制备抗氧化成分的方法包括如下步骤：
(1)选取无病虫损害的茶籽皮(将油茶榨油剩下的茶籽皮筛去严重病虫害的茶壳，剔除茶籽皮中被虫蛀、坏掉部分)，粉碎，过50—100目筛，得茶籽皮粉，备用；
(2)用正己烷或石油醚回流提取茶籽皮粉，提取液过滤，除去茶籽皮中的油脂类成分，得脱脂茶籽皮滤渣；
(3)向茶籽皮滤渣中加入1,3-丁二醇溶剂，搅拌提取2—6h，得提取液，备用；所述1,3-丁二醇溶剂的质量为茶籽皮滤渣质量的5—12倍；重复该步骤2—3次，将每次所得提取液分别进行下一步骤的处理或合并后统一进行下一步骤的处理；
(4)通过蝶式离心方式过滤步骤(3)所得的提取液，去除提取液中的颗粒物质，得A滤液，备用；
(5)通过膜分离方式去除步骤(4)所得滤液中的大分子物质(多糖、蛋白等)，收集膜分离处理后的B滤液，所述B滤液中即含抗氧化成分，颜色澄清，可直接用于化妆品原料
优选地，步骤(2)回流提取时正己烷或石油醚的质量为茶籽皮粉质量的2倍，回流提取温度≤55℃。步骤(3)所述1,3-丁二醇溶剂的质量百分比浓度为35—80％，搅拌提取的温度≤55℃。步骤(5)所述膜分离方式是采用陶瓷膜，所述陶瓷膜的孔径为100—200nm，膜分离温度≤55℃。
本发明直接以1,3-丁二醇溶液做溶剂，由于用1,3-丁二醇溶液做溶剂，通过调节1,3-丁二醇与H2O的比例，使溶剂形成的空穴有利于酚类物质的进入，提高了提取效率和选择性。1,3-丁二醇在化妆品中常做为保湿剂，可以在化妆品中安全使用，不需要从提取物中脱除，减少了传统方法的溶剂脱除、干燥过程的能耗，也减少了这些工艺过程对抗氧化性能的破坏。与已有技术相比，本发明的茶籽皮提取物做为化妆品原料在抗氧化能力、能耗、工艺的简化、微生物洁净度等方面具有显著优势。
附图说明
图1为Trolox抗氧化能力的标准曲线。
具体实施方式
实施例1
1.选取无病虫损害的茶籽皮，粉碎过筛，称取3kg待用；
2.步骤1中茶籽皮粉末，加入6L的正己烷回流提取2h，提取液过滤，留取滤渣待用；
3.往步骤2中脱脂茶籽皮粉末中，加入15L浓度为40％的1.3-丁二醇溶液，搅拌提取3h,提取温度55℃，提取液过滤；
4.收集步骤3的提取液，依次通过离心机，膜分离设备，得到澄清液体(B滤液)11.3L，可直接添加至化妆品原料中。
实施例2
1.选取无病虫损害的茶籽皮，粉碎过100目筛，称取3kg待用；
2.步骤1中茶籽皮粉末，加入6L的正己烷回流提取2h，提取液过滤，留取滤渣待用；
3.往步骤2中脱脂茶籽皮滤渣中，加入浓度为60％的1,3-丁二醇25L，搅拌提取2h，提取温度45℃，提取液过滤待用；
4.收集步骤3的提取液，通过管式分离机，除去大颗粒沉淀，后通过膜分离设备进行纯化，得到澄清液体(B滤液)21.7L，可直接作为原料添加至化妆品中。
实施例3
1.选取无病虫损害的茶籽皮，粉碎过100目筛，称取3kg待用；
2.步骤1中茶籽皮粉末，加入6L的石油醚回流提取2h，提取液过滤，留取滤渣晾干待用；
3.往步骤2中脱脂茶籽皮滤渣中，加入浓度为50％的的1,3-丁二醇溶液30L，搅拌提取2h，提取温度50℃，提取液过滤；
4.收集步骤3的提取液，通过蝶式离心分离、初步分离，去除大颗粒沉淀，然后通过陶瓷膜分离设备进行初步纯化，得到澄清液体(B滤液)26.2L,可直接作为原料添加至化妆品中。
将本发明中所得茶籽皮提取液(B滤液)进行抗氧化性实验，相关实验步骤和结果如：抗氧化性测定
本发明中采用ABTS总抗氧化能力测定法来测定茶籽皮的抗氧化性。ABTS，化学全称2,2'-联氮双(3-乙基苯并噻唑啉-6-磺酸)二铵盐。ABTS与强氧化剂过硫酸钾反应生成蓝绿色阳离子自由基ABTS·+，该阳离子自由基稳定，在734nm处有紫外吸收峰。当有抗氧化剂存在，会与ABTS·+自由基发生反应，使紫外吸收减弱，蓝绿色减褪，吸光度值减小。利用其吸光度与浓度呈定量关系，可以通过体系在734nm处的吸光度反应样品的总抗氧化性能力。这种方法操作简便，方便测量，一般采用Trolox(水溶性VE)作为对照。
1.ABTS工作液的配制
本实验采用ABTS试剂盒，试剂盒中包括ABTS[2,2-联氮-二(3-乙基-苯并噻唑-6-磺酸)二铵盐]溶液，氧化剂溶液，Trolox(水溶性维生素E)溶液。移取40ulABTS溶液、40ul氧化剂溶液，混匀后，配置成ABTS母液，室温避光存放12小时；在使用前，用丁二醇稀释成ABTS工作液，测量其吸光度，在0.7±0.05范围内方可使用。
2.Trolox标准曲线的测定
将ABTS试剂盒中自带的Trolox标准溶液(10mM)，用丁二醇配置成1、1.5、3、6、9mM浓度的系列标准品溶液，在96孔板的每个检测孔中加入200μL的ABTS工作液，空白对照孔中加入10μl的丁二醇溶液，标准曲线孔中加入各浓度的Trolox标准溶液，混合均匀，室温孵育2min后，用酶标仪测定734nm处的吸光度，测出对照品清除率关于浓度的标准曲线如图1所示。
Trolox清除率＝(A0-AX)/A0×100％(A0：空白对照，Ax：Trolox的吸光度)
3.样品总抗氧化能力的测定
预实验：96孔板中加入200μL的ABTS工作液，滴加实施例1中B滤液10μL，摇匀后测定吸光度，根据清除率确定实验中茶籽皮浓度范围。本实验中浓度范围为0.1、0.25、0.5、1.05、2.1mg/mL。
将实施例1中B滤液稀释到以上浓度，在96孔板的样品检测孔内加入10μL各浓度B滤液，空白对照孔中加入10μL的1,3-丁二醇溶液，混匀后，室温孵育2min，使用酶标仪测定734nm处的吸光度，并计算B滤液的半数清除浓度(IC50)，如下表1所示。
表-1 B滤液半数清除浓度
由结果可知，B滤液的半数清除浓度远小于水溶性VE，说明B滤液的总抗氧化能力远高于水溶性VE。
微生物限度检查
1.仪器
2.培养基
3.大肠埃希菌检查
3.1供试液制备
取B滤液(以下称“本品”)10ml，加pH7.0无菌氯化钠-蛋白胨缓冲液至100ml，混匀，制成1:10的供试液，备用。
3.2试验组
取上述1:10的供试液10ml接种至100ml胰酪大豆胨液体培养基中，再加入大肠埃希菌菌悬液1ml(<100cfu)，35℃培养24小时；取上述培养物1ml接种至100ml麦康凯液体培养基中，42℃培养48小时；取麦康凯液体培养物划线接种于麦康凯琼脂平板上，35℃培养72小时，观察结果。
3.3供试品组
除不加试验菌菌悬液，其他同试验组。
3.4阳性对照试验
除不加供试液，其他操作同试验组。
3.5阴性对照组
不加试验菌，且用10ml pH7.0无菌氯化钠-蛋白胨缓冲溶液代替供试液，其他同试验组进行操作。
3.6结果
备注：“+”表示阳性或典型菌落生长，“-”表示阴性或无菌生长。
上述试验结果表明：本品大肠埃希菌未检出。
4.金黄色葡萄球菌检查
4.1供试液制备
取本品10ml，加pH7.0无菌氯化钠-蛋白胨缓冲液至100ml，混匀，制成1:10的供试液，备用。
4.2试验组
取上述1:10的供试液10ml接种至100ml胰酪大豆胨液体培养基中，再加入金黄色葡萄球菌菌悬液1ml(<100cfu)，35℃培养24小时；取上述培养物划线接种于甘露醇氯化钠琼脂平板上，35℃培养72小时，观察结果。
4.3供试品组
除不加试验菌菌悬液，其他同试验组。
4.4阳性对照组
除不加供试液，其他操作同试验组。
4.5阴性对照组
不加试验菌，且用10ml pH7.0无菌氯化钠-蛋白胨缓冲溶液代替供试液，其他同试验组进行操作。
4.6结果
备注：“+”表示阳性或典型菌落生长，“-”表示阴性或无菌生长。
上述试验结果表明：本品金黄色葡萄球菌未检出。
Claims (4)
1.一种以1,3-丁二醇为溶剂从油茶茶籽皮中提取抗氧化成分的方法，其特征在于，所述方法包括如下步骤：
(1)选取无病虫损害的茶籽皮，粉碎，过50—100目筛，得茶籽皮粉，备用；
(2)用正己烷或石油醚回流提取茶籽皮粉，提取液过滤，除去茶籽皮中的油脂类成分，得脱脂茶籽皮滤渣；
(3)向茶籽皮滤渣中加入1,3-丁二醇溶剂，搅拌提取2—6h，得提取液，备用；所述1,3-丁二醇溶剂的质量为茶籽皮滤渣质量的5—12倍；重复该步骤2—3次，将每次所得提取液分别进行下一步骤的处理或合并后统一进行下一步骤的处理；
(4)通过蝶式离心方式过滤步骤(3)所得的提取液，去除提取液中的颗粒物质，得A滤液，备用；
(5)通过膜分离方式去除步骤(4)所得滤液中的大分子物质，收集膜分离处理后的B滤液，所述B滤液中即含抗氧化成分。
2.如权利要求1所述的方法，其特征在于，步骤(2)回流提取时正己烷或石油醚的质量为茶籽皮粉质量的2倍，回流提取温度≤55℃。
3.如权利要求1所述的方法，其特征在于，步骤(3)所述1,3-丁二醇溶剂的质量百分比浓度为35—80％，搅拌提取的温度≤55℃。
4.如权利要求1所述的方法，其特征在于，步骤(5)所述膜分离方式是采用陶瓷膜，所述陶瓷膜的孔径为100—200nm，膜分离温度≤55℃。
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| CN107198668A (zh) * | 2017-05-25 | 2017-09-26 | 中南大学 | 油茶籽皮中抗氧化成分提取物及其提取方法和应用 |
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| CN115192638B (zh) * | 2022-08-31 | 2023-09-01 | 北京尚捷优蓝科技有限公司 | 一种大花黄牡丹抗氧化活性部位及其制备方法和应用 |
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