CN113549497A - 一种超声辅助天然深共晶溶液提取紫苏叶精油的方法以及紫苏叶精油的应用 - Google Patents
一种超声辅助天然深共晶溶液提取紫苏叶精油的方法以及紫苏叶精油的应用 Download PDFInfo
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Abstract
本发明公开了一种超声辅助天然深共晶溶液提取紫苏叶精油的方法以及紫苏叶精油的应用。本发明由不同成分组成的天然深共晶溶液(组分包括：氯化胆碱、柠檬酸、苹果酸、D‑葡萄糖、D‑果糖)提取了天然紫苏叶精油(得率约为0.5％‑0.7％)，并将其与超声辅助传统水蒸气蒸馏的紫苏叶精油(得率约为0.21％)作对比，证明经由超声辅助天然深共晶溶液提取方法，紫苏叶精油的得率提高，提取所得的紫苏叶精油具有更强的抗氧化性，并且对于大肠杆菌、金黄色葡萄球菌、白色念珠菌和黑曲霉菌有更好的抑制效果。因此，超声辅助天然深共晶溶液提取可以作为一种新型的提取方法在天然香原料提取领域中应用。
Description
技术领域
本发明涉及一种超声辅助天然深共晶溶液提取紫苏叶精油的方法以及紫苏叶精油的应用，属于天然产物技术领域。
背景技术
天然香原料主要指用一定方法从植物的根、茎、叶、花、果实或者动物中提取得到含香物质，由于其气味天然多韵，且含有丰富的生物活性成分，被广泛应用于香料香精、日化、食品以及生物领域。天然香原料根据提取方法的不同所得到的产物不同：精油是由水蒸气蒸馏含香的天然原料得到的油状挥发性混合物；净油是用溶剂浸提天然香原料得到浸膏后，经过冷冻、乙醇溶解提取而得到的物质；也有经水提、醇提法后由大孔树脂吸附洗脱等分离手法得到多酚、多糖类物质。天然香原料取材天然，成分复杂多样，香气非单一人工香原料可模拟。在合成香料发展日益壮大的今日，天然香原料仍然具有不可替代的优势，而精油则是其中具有代表性的一类。
传统的天然香原料提取主要有水蒸气蒸馏法、溶剂浸提法、冷榨法；现今，分子蒸馏法、固相微萃取法、超临界流体萃取法也正在日趋优化。辅助方法有且不限于微波辅助、超声辅助、闪式提取前处理等。传统的水蒸气蒸馏提取方法效率低，天然深共晶溶液是离子液体的一种，其成分来自生物体的代谢物，不仅具有离子液体溶解能力强、形状可设计、导电、制备简易的特点，而且具有良好的生物相容性和降解性。目前已有关于天然深共晶溶剂用于提取天然产物中的有效活性成分的相关研究和报道，且显示提取效率高于一般的提取方法。但是目前并没有应用到紫苏叶精油的提取工艺中。
紫苏叶精油的主要成分是单萜类、倍半萜类及其含氧化合物；根据紫苏叶化学型的不同，其精油主要成分种类不同。紫苏叶精油具有较好的抗菌、消炎性，也可舒缓人的抑郁情绪起镇静作用；也有研究将紫苏叶精油应用于食品防腐和风味添加方面。目前未见超声提取-天然深共晶溶液辅助水蒸气蒸馏得到紫苏叶精油的相关报道。
发明内容
本发明所要解决的技术问题是：采用传统的水蒸气蒸馏的方法从紫苏叶中提取紫苏精油的效率低等问题。
为了解决上述技术问题，本发明提供了一种超声辅助天然深共晶溶液提取紫苏叶精油的方法，包括：以天然深共晶溶液替代水作为提取溶剂，加入紫苏叶粉末进行混合后超声处理，最后采用水蒸气蒸馏蒸出紫苏叶精油。
优选地，所述的天然深共晶溶液为氯化胆碱与D-葡萄糖的水溶液、氯化胆碱与柠檬酸的水溶液、氯化胆碱与苹果酸的水溶液、D-果酸与苹果酸的水溶液或D-葡萄糖与柠檬酸的水溶液。
优选地，所述的紫苏叶粉末与天然深共晶溶液的质量比为1:4～1:8；所述水蒸气蒸馏的时间为2～4h。
优选地，所述的天然深共晶溶液的质量浓度为60％。
优选地，所述的氯化胆碱与D-葡萄糖的摩尔比为3:1；所述的氯化胆碱与柠檬酸的摩尔比为1:1；所述的氯化胆碱与苹果酸的摩尔比为2:1；所述的D-果酸与苹果酸的摩尔比为1:2；所述的D-葡萄糖与柠檬酸的摩尔比为2:1。
本发明还提供了上述的超声辅助天然深共晶溶液提取紫苏叶精油的方法提取所得的紫苏叶精油，所述的紫苏叶精油的成分包括单萜类化合物、含氧单萜类化合物、倍半萜类化合物、含氧倍半萜类化合物、含氧双萜类化合物、脂肪族类化合物和芳香族类化合物。
本发明还提供了上述的超声辅助天然深共晶溶液提取紫苏叶精油的方法提取所得的紫苏叶精油在制备抗氧化用品和/或抑菌用品中的应用。
与现有技术相比，本发明的有益效果在于：
1.本发明的超声辅助天然深共晶溶液提取紫苏叶精油的方法相较于传统水蒸气蒸馏法提取率更高，提取率在0.5～0.7％，是传统方法的2～3倍；且本发明提取所得的紫苏叶精油中活性物质种类更多，抗氧化性能更好；
2.本发明的方法相较于传统水蒸气蒸馏方法提取所得的紫苏叶精油，对于大肠杆菌、金黄色葡萄球菌、白色念珠菌和黑曲霉菌等菌种的抑菌圈直径更大，最小抑菌浓度更小，抑菌效果更好。
具体实施方式
为使本发明更明显易懂，兹以优选实施例作详细说明如下。
实施例1
一种超声辅助天然深共晶溶液提取紫苏叶精油的方法，包括如下步骤：
(1)选用氯化胆碱与D-葡萄糖作为天然深共晶组成成分，氯化胆碱：D-葡萄糖的摩尔比分别为1:1、1:2、2:1、1:3、3:1，共72g，加入48g去离子水，45℃下混合搅拌至澄清透明。
(2)各取20g干紫苏叶粉加入到120g上述五组制备的天然深共晶溶液中，600W超声提取5min后加水至溶液总体积800mL，后继续600W超声混合20min。最终进行水蒸气蒸馏3h，蒸出紫苏叶精油。
其中，氯化胆碱：D-葡萄糖摩尔比3:1条件下提取的紫苏叶精油得率最高，为0.57％，后续的测试试验采用此条件下所得紫苏叶精油进行测试。
实施例2
一种超声辅助天然深共晶溶液提取紫苏叶精油的方法，包括如下步骤：
(1)选用氯化胆碱与柠檬酸作为天然深共晶组成成分，氯化胆碱：柠檬酸的摩尔比分别为1:1、1:2、2:1、1:3、3:1，共72g，加入48g去离子水，45℃下混合搅拌至澄清透明。
(2)各取20g干紫苏叶粉加入到120g上述五组制备的天然深共晶溶液中，600W超声提取5min后加水至溶液总体积800mL，后继续600W超声混合20min。最终进行水蒸气蒸馏3h，蒸出紫苏叶精油。
其中，氯化胆碱：柠檬酸摩尔比1:1条件下提取的紫苏叶精油得率最高，为0.61％，后续的测试试验采用此条件下所得紫苏叶精油进行测试。
实施例3
一种超声辅助天然深共晶溶液提取紫苏叶精油的方法，包括如下步骤：
(1)选用氯化胆碱和苹果酸作为天然深共晶组成成分，氯化胆碱：苹果树的摩尔比分别为1:1、1:2、2:1、1:3、3:1，共72g，加入48g去离子水，45℃下混合搅拌至澄清透明。
(2)各取20g干紫苏叶粉加入到120g上述五组制备的天然深共晶溶液中，600W超声提取5min后加水至溶液总体积800mL，后继续600W超声混合20min。最终进行水蒸气蒸馏3h，蒸出紫苏叶精油。
其中，氯化胆碱：苹果酸摩尔比2:1条件下提取的紫苏叶精油得率最高，为0.63％，后续的测试试验采用此条件下所得紫苏叶精油进行测试。
实施例4
一种超声辅助天然深共晶溶液提取紫苏叶精油的方法，包括如下步骤：
(1)选用D-果糖和苹果酸作为天然深共晶组成成分，D-果糖：苹果酸的摩尔比分别为1:1、1:2、2:1、1:3、3:1，共72g，加入48g去离子水，45℃下混合搅拌至澄清透明。
(2)各取20g干紫苏叶粉加入到120g上述五组制备的天然深共晶溶液中，600W超声提取5min后加水至溶液总体积800mL，后继续600W超声混合20min。最终进行水蒸气蒸馏3h，蒸出紫苏叶精油。
其中，D-果糖：苹果酸摩尔比1:2条件下提取的紫苏叶精油得率最高，为0.57％，后续的测试试验采用此条件下所得紫苏叶精油进行测试。
实施例5
一种超声辅助天然深共晶溶液提取紫苏叶精油的方法，包括如下步骤：
(1)选用D-葡萄糖和柠檬酸作为天然深共晶组成成分，D-葡萄糖：柠檬酸的摩尔比分别为1:1、1:2、2:1、1:3、3:1，共72g，加入48g去离子水，45℃下混合搅拌至澄清透明。
(2)各取20g干紫苏叶粉加入到120g上述五组制备的天然深共晶溶液中，600W超声提取5min后加水至溶液总体积800mL，后继续600W超声混合20min。最终进行水蒸气蒸馏3h，蒸出紫苏叶精油。
其中，D-葡萄糖：柠檬酸摩尔比2:1条件下提取的紫苏叶精油得率最高，为0.69％，后续的测试试验采用此条件下所得紫苏叶精油进行测试。
对比例
一种超声辅助水蒸气蒸馏提取紫苏叶精油的方法：
干紫苏叶粉20g与水780g混合和，600W超声辅助提取20min，进行水蒸气蒸馏得紫苏叶精油，得率为0.21％。
测试试验：
一、采用GC-MS分析实施例1～5和对比例提取所得的紫苏叶精油中的成分：
GC-MS条件：惠普7890气相色谱与惠普5975C四级杆质谱联用，气象色谱柱型号：安捷伦HP-INNOWAX(60m×250μm×0.25μm)。氦气作为载气，流速1mL/min。分流比为10:1。升温程序：初始温度50℃维持3min后以8℃/min升温至115℃；再以3℃/min至200℃，保持3min；最终以4℃/min升温至230℃，保留10min。GC-MS检测结果如表1所示。
表1 GC-MS检测结果
由表1可知，紫苏叶精油中主要成分为紫苏醛和β-石竹烯；主要成分种类有萜类、脂肪类、芳香族类；经由天然深共晶溶液辅助提取的紫苏叶精油保留了紫苏叶精油的主要成分，且含氧单萜类、含氧倍半萜、脂肪族类和芳香族类化合物种类明显增多。
二、紫苏叶精油的总酚含量及抗氧化性测定：
采用福林酚法测定实施例和对比例所得紫苏叶精油的总酚含量；采用DPPH、ABTS法检测实施例和对比例所得紫苏叶精油的抗氧化性，并测定各紫苏叶精油的IC50值。紫苏叶精油的总酚含量及抗氧化性结果如表2所示。
表2 紫苏叶精油总酚含量及抗氧化性能指标
三、紫苏叶精油抑菌性实验
采用滤纸片法分别测定了实施例和对比例所得精油在不同浓度下对于大肠杆菌、金黄色葡萄球菌、白色念珠菌和黑曲霉菌的抑菌圈直径并确定了各实施例精油的最小抑菌浓度。抑菌性实验结果如表9所示。
表9不同浓度紫苏叶精油的抑菌圈直径和最小抑菌浓度
由表9可知，经由超声-天然深共晶溶液提取后的紫苏叶精油相较于超声-水蒸气蒸馏方法所得精油，抑菌圈直径更大，最小抑菌浓度更小，对于所选菌种的抑菌效果更好。
上述实施例仅为本发明的优选实施例，并非对本发明任何形式上和实质上的限制，应当指出，对于本技术领域的普通技术人员，在不脱离本发明的前提下，还将可以做出若干改进和补充，这些改进和补充也应视为本发明的保护范围。
Claims (7)
1.一种超声辅助天然深共晶溶液提取紫苏叶精油的方法，其特征在于，包括：以天然深共晶溶液替代水作为提取溶剂，加入紫苏叶粉末进行混合后超声处理，最后采用水蒸气蒸馏蒸出紫苏叶精油。
2.根据权利要求1所述的超声辅助天然深共晶溶液提取紫苏叶精油的方法，其特征在于，所述的天然深共晶溶液为氯化胆碱与D-葡萄糖的水溶液、氯化胆碱与柠檬酸的水溶液、氯化胆碱与苹果酸的水溶液、D-果酸与苹果酸的水溶液或D-葡萄糖与柠檬酸的水溶液。
3.根据权利要求1所述的超声辅助天然深共晶溶液提取紫苏叶精油的方法，其特征在于，所述的紫苏叶粉末与天然深共晶溶液的质量比为1:4～1:8；所述水蒸气蒸馏的时间为2～4h。
4.根据权利要求1所述的超声辅助天然深共晶溶液提取紫苏叶精油的方法，其特征在于，所述的天然深共晶溶液的质量浓度为60％。
5.根据权利要求2所述的超声辅助天然深共晶溶液提取紫苏叶精油的方法，其特征在于，所述的氯化胆碱与D-葡萄糖的摩尔比为3:1；所述的氯化胆碱与柠檬酸的摩尔比为1:1；所述的氯化胆碱与苹果酸的摩尔比为2:1；所述的D-果酸与苹果酸的摩尔比为1:2；所述的D-葡萄糖与柠檬酸的摩尔比为2:1。
6.权利要求1～5中任意一项所述的超声辅助天然深共晶溶液提取紫苏叶精油的方法提取所得的紫苏叶精油，其特征在于，所述的紫苏叶精油的成分包括单萜类化合物、含氧单萜类化合物、倍半萜类化合物、含氧倍半萜类化合物、含氧双萜类化合物、脂肪族类化合物和芳香族类化合物。
7.权利要求1～5中任意一项所述的超声辅助天然深共晶溶液提取紫苏叶精油的方法提取所得的紫苏叶精油在制备抗氧化用品和/或抑菌用品中的应用。
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Application publication date: 20211026 |