CN104490994A - 一种从迷迭香中提取脂溶性和水溶性抗氧化剂的方法 - Google Patents
一种从迷迭香中提取脂溶性和水溶性抗氧化剂的方法 Download PDFInfo
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Abstract
本发明提供了一种从迷迭香中提取脂溶性和水溶性抗氧化剂的方法，包括以下步骤：（1）将采收的迷迭香植物嫩茎及叶片自然荫干；（2）对自然荫干的迷迭香进行水蒸气蒸馏，得到迷迭香精油和残留物；（3）对提取精油后残留物进行粉碎，加入一定浓度的乙醇溶液，超声辅助提取数次，提取后进行离心分离，得到浸提液，合并浸提液；（4）对浸提液进行脱色处理，在浸提液中加入一定量活性白土，一定温度下搅拌维持一段时间，去除活性白土得到脱色浸提液；（5）将脱色浸提液进行真空浓缩至一定体积，析出沉淀；（6）浓缩液离心得到沉淀和水相部分；（7）分别将沉淀和水相部分进行真空干燥，得到脂溶性抗氧化剂和水溶性抗氧化剂。
Description
技术领域
本发明涉及迷迭香的多种活性成分的综合提取方法，尤其是从迷迭香原料中提取脂溶性和水溶性抗氧化剂的方法。
技术背景
迷迭香，别名艾菊，属唇形科亚灌木或多年生草本香料植物，原产于地中海地区，我国于20世纪70年代末成功引种，随后在全国各地推广。除了可用做迷迭香主要用于提取精油和抗氧化剂。迷迭香精油是传统的天然香料，同时还有一定的天然防腐作用和临床功效，其成分在医药保健方面的功能，如消炎、抗肿瘤、抗癌、治疗心血管疾病、保肝降酶等等方面也受到了国内外广大学者和科研工作者的极大关注。迷迭香抗氧化产品种类多，包括鼠尾草酚、迷迭香酚、迷迭香酸、鼠尾草酸、熊果酸等，其中二萜酚酸类是迷迭香中主要的抗氧化活性成分。迷迭香抗氧化因其独特的抗氧化性能——安全、高效、耐热、广谱，而代替人工抗氧化剂 BHA、BHT、TBHQ等成为近年来食品、日用化工、医药保健方面研究开发的重点之一。
目前迷迭香精油主要使用传统水蒸气蒸馏法提取，近期也有使用CO2超临界萃取的报道。迷迭香抗氧化剂则主要采取食用油脂、有机溶剂、超临界CO2超临界萃取、碱水和过热水等进行提取，也可以综合使用几种提取方法。从迷迭香中提取抗氧化剂的生产工艺主要存在下列不足:（1）现有的某些工艺过程中需进行超临界萃取、冷冻分离或冷冻干燥，其设备投资大，导致生产成本高；（2）大部分生产工艺一般仅得到混合抗氧化剂，未进一步对其再分离，导致产品单一，且不能水溶或脂溶完全，限制了该抗氧化剂的应用范围，资源附加值低；（3）脱色效果不佳，导致产品颜色为黒黄色；（4）已有工艺在实际生产应用方面的不合理性：一是过程中有些使用卤代烃、丙酮或甲醇等有机溶剂提取抗氧化剂，这些溶剂对操作人员身体有害，产品中微量的溶剂残留对人体有害；二是有些技术中使用酸或碱液，酸碱会导致迷迭香中部分有效成分的破坏，如苷类物质在酸或碱性条件下易水解，黄酮类化合物在碱性条件下易降解而失去抗氧化活性。
脱色分为吸附脱色和化学脱色，油脂预处理一般采用吸附脱色。脱色效果的好坏直接影响到产品质量和成本，因此选择适宜的吸附剂极其重要。常用的吸附剂有活性炭和白土。活性炭作为吸附剂能够选择性地吸附色素和臭味物质，但活性炭吸附剂价格昂贵、油率高。白土又称漂土，经酸化处理后其表面积大大增加，吸附性能大大提高，这种白土称为活性白土 (或称酸性白土)。白土是油脂精炼时常用的脱色剂。活性白土较天然白土的k值大，故本实验采用活性白土作为脱色剂。
发明内容
本发明的目的在于克服了已有工艺的缺点，提供一种从迷迭香中提取脂溶性和水溶性抗氧化剂的方法，具有得率高、原料利用充分、生产成本低等优点，同时大幅改善了迷迭香抗氧化剂产品的应用性能，提高了迷迭香附加值。
为达到上述目的，本发明提供一种从迷迭香中提取脂溶性和水溶性抗氧化剂的方法，包括如下步骤：
（1）将采收的迷迭香植物嫩茎及叶片自然荫干；
（2）对自然荫干的迷迭香进行水蒸气蒸馏1～3小时，得到迷迭香精油和残留物；
（3）对提取精油后残留物进行粉碎，加入8～12倍（相对干迷迭香）的50%乙醇溶液，然后超声波辅助提取1～3次，提取后进行离心分离，得到浸提液，合并浸提液；
（4）对浸提液进行脱色处理，在浸提液中加入1～10%活性白土，50～100 ℃条件下搅拌维持20～50 min，去除活性白土得到脱色浸提液；
（5）将脱色浸提液进行真空浓缩，体积浓缩至10～20%，析出大量沉淀；
（6）浓缩液于4000 r/min条件下离心10～20 min得到沉淀和水相部分；
（7）分别将沉淀和水相部分进行真空干燥，得到脂溶性抗氧化剂和水溶性抗氧化剂。
本工艺设备简单，投资少，脱色效果显著，适合工业化生产。所得产品成本低，得率高，脂溶性和水溶性好，用途广泛。
具体实施方式
下面通过实施例对本发明进行具体描述，以下实施例只用于对本发明进一步说明，不能理解为对本发明保护范围的限定。
实施例1：一种从迷迭香中提取脂溶性和水溶性抗氧化剂的方法，包括以下步骤：
（1）原料为河南省民权县生产的迷迭香，将采收的迷迭香植物嫩茎及叶片自然荫干，然后取100 g水蒸气蒸馏3小时，得到迷迭香精油和残留物；对提取精油后残留物进行粉碎，加入10倍（相对干迷迭香）的50%乙醇溶液，然后超声波辅助提取2次，合并两次离心得到的浸提液；在浸提液中加入4%活性白土，55 ℃条件下搅拌维持30 min，去除活性白土得到脱色浸提液；将脱色浸提液进行真空浓缩，体积浓缩至10%，析出大量沉淀；浓缩液于4000 r/min条件下离心15 min得到沉淀和水相部分；分别将沉淀和水相部分进行真空干燥，得到脂溶性抗氧化剂鼠尾草酸5.64 g和水溶性抗氧化剂9.78 g，得率分别为5.64%和9.78%，总抗氧化剂得率为15.42%。
实施例2～5 ：
本实施例的提取方法与实施例1基本相同，区别在于：将活性土加入量由4%改换为2%（例2），6%（例3），8%（例4），10%（例5）。例1～5在于说明不同比例的活性白土对色素的消除及终产品得率的影响。计算例2～5中抗氧化剂的得率并同例1相比较，结果如表1。
表1 不同活性白土加入量对色素的消除、产物利率的影响
| 活性白土加入量(%) | 水溶性抗氧化剂得率(%) | 脂溶性抗氧化剂利率（%） | 脱色效果及产品颜色 | 总抗氧化得率（%） |
| 2% | 10.02 | 6.17 | 差，淡绿色/黄绿色 | 16.19 |
| 6% | 9.34 | 5.69 | 一般，淡绿色/淡黄色 | 15.03 |
| 8% | 8.86 | 5.36 | 好，淡绿色/黄色 | 14.22 |
| 10% | 8.37 | 4.81 | 好，淡绿色/暗黄色 | 13.18 |
| 4% | 9.78 | 5.94 | 一般，淡绿色/黄绿色 | 15.72 |
Claims (3)
1.一种从迷迭香中提取脂溶性和水溶性抗氧化剂的方法，其特征在于包括以下步骤：（1）将采收的迷迭香植物嫩茎及叶片自然荫干；（2）对自然荫干的迷迭香进行水蒸气蒸馏1～3小时，得到迷迭香精油和残留物；（3）对提取精油后残留物进行粉碎，加入8～12倍（相对干迷迭香）的50%乙醇溶液，然后超声波辅助提取1～3次，提取后进行离心分离，得到浸提液，合并浸提液；（4）对浸提液进行脱色处理，在浸提液中加入1～10%活性白土，50～100 ℃条件下搅拌维持20～50 min，去除活性白土得到脱色浸提液；（5）将脱色浸提液进行真空浓缩，体积浓缩至10～20%，析出沉淀；（6）浓缩液于4000 r/min条件下离心10～20 min得到沉淀和水相部分；（7）分别将沉淀和水相部分进行真空干燥，得到脂溶性抗氧化剂和水溶性抗氧化剂。
2.根据权利要求 1 所述的制备方法，其特征在于，所述步骤（4）中，对浸提液进行脱色处理，所用脱色剂为活性白土。
3.根据权利要求 1 所述的制备方法，其特征在于，所述步骤（4）中，对浸提液脱色处理条件为：活性白土量为1～10%，脱色温度为30～100 ℃，时间为20～50 min。
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