CN109651127A - 一种斑点叉尾鮰鱼内脏油dha和epa的分离纯化方法 - Google Patents
一种斑点叉尾鮰鱼内脏油dha和epa的分离纯化方法 Download PDFInfo
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Abstract
本发明提供了一种斑点叉尾鮰鱼内脏油DHA和EPA的分离纯化方法，包括以下步骤：(1)粗鱼油的制备：处理过的斑点叉尾鮰内脏经过解冻后，放入具塞锥形瓶中，加入蒸馏水，然后用KOH调节pH值，并向锥形瓶中填充氮气，进行第一次恒温水解，加入氯化钾，继续进行第二次恒温水解，在5000g的离心力作用下，趁热离心10min，分离出上层粗鱼油；(2)粗鱼油的预处理：将上述步骤制取的粗鱼油加入乙醇和浓硫酸，加热回流；将馏出物用足量的正己烷进行萃取；萃取物通过硅胶层析法，进行分离。本发明提供的分离纯化方法实现了水产品副产物的高值化利用，解决了水产品副产物资源的综合利用问题，提高了水产品加工的附加值；且具有工序简单、易实现工业化生产的特点。
Description
技术领域
本发明涉及风味酱技术领域，具体涉及一种斑点叉尾鮰鱼内脏油DHA和EPA的分离纯化方法。
背景技术
目前，随着我国淡水鱼产量和加工规模的不断提高，加工下脚料也越来越多，主要包括鱼头、鱼骨、鱼皮、鱼内脏及其残余碎肉等。这些下脚料除大部分被用作饲料鱼粉外，剩余部分只能被随意丢弃和掩埋。
几乎所有的鱼油中均含有以DHA、EPA为代表的多不饱和脂肪酸，DHA、EPA具有作为人体必需的脂肪酸，具有降低患心血管疾病、保护视力、缓解抑郁、健脑益智等功效。本发明采用鮰鱼加工副产物鮰鱼内脏为原料，提取粗鱼油，进而制备高附加值的产品EPA、DHA，不仅有助于保护环境，而且对于合理利用资源，提高水产品加工附加值均有重要的意义。
上海水产加工技术中心利用鱿鱼内脏自身酶水解内脏及其它废物，开发出鱿鱼油、内脏水解液做为调味道品原料或氨基酸添加剂。鱼油提取率最高为24.8％，胶状物提取率为7.8％。
华南理工大学食品与生物工程学院通过以淡水鱼内脏生产鱼油，经121℃蒸煮1.5h，用20ml/L，浓度为0.01g/L的柠檬酸水溶液酸洗，温度为80℃，真空度0.095Mpa真空干燥，填加0.2g/L的TBHQ与柠檬酸钠(2∶1)的混合物等可控鱼油异味产生。
南京化工大学、江苏省淡水水产研究所采用添加混合抗氧化剂的方法及酶解法提取鱼内脏油技术，真空水蒸气脱臭法鱼油精制技术及综合法和CO2超临界流体萃取技术，使EPA、DHA总含量达82.0％以上。
发明内容
本发明的目的在于提供一种斑点叉尾鮰鱼内脏油DHA和EPA的分离纯化方法，制备得到的风味酱具有很高的营养价值，可以调节血脂、预防老年痴呆、提高记忆力、提高免疫力。
为实现上述目的，本发明提供了一种斑点叉尾鮰鱼内脏油DHA和EPA的分离纯化方法，包括以下步骤：
(1)粗鱼油的制备：处理过的斑点叉尾鮰内脏经过解冻后，放入具塞锥形瓶中，加入蒸馏水，然后用KOH调节pH值，并向锥形瓶中填充氮气，进行第一次恒温水解，加入氯化钾，继续进行第二次恒温水解，在5000g的离心力作用下，趁热离心10min，分离出上层粗鱼油；
(2)粗鱼油的预处理：将上述步骤制取的粗鱼油加入乙醇和浓硫酸，加热回流；将馏出物用足量的正己烷进行萃取；萃取物通过硅胶层析法，进行分离；
其中，粗鱼油进行三步真空分子蒸馏，温度分阶段分别截取在65-70℃、100-105℃、120-125℃三个温度段上截止轻馏分、中间馏分、重组分。
进一步地，所述加入蒸馏水后液料比1-2mL:1g。
进一步地，所述KOH的浓度为20％。
进一步地，所述pH值为6.0-7.0。
进一步地，所述第一次恒温水解的时间为30-300min。
进一步地，所述氯化钾的加入量为0.5-100g。
进一步地，所述乙醇为足量。
进一步地，所述浓硫酸为10-200mL。
进一步地，所述第二次恒温水解的时间为30-300min。
进一步地，所述蒸馏的真空度控制在2-4mmHg。
本发明的优点在于：
1、实现了水产品副产物的高值化利用，解决了水产品副产物资源的综合利用问题，提高了水产品加工的附加值；
2、本方法分离DHA、EPA具有工序简单、易实现工业化生产的特点；
3、本方法分离出DHA、EPA纯度高达90％，DHA:EPA＝3：2，且产品风味独特，无异味。
具体实施方式
下面结合具体实施方式对本发明做进一步说明，以下实施例旨在说明本发明而不是对本发明的进一步限定。
本发明所采用的原料均能够从市场上购买或按照现有技术合成。
实施例1
一种斑点叉尾鮰鱼内脏油DHA和EPA的分离纯化方法，包括以下步骤：
(1)粗鱼油的制备：处理过的斑点叉尾鮰内脏经过解冻后，放入具塞锥形瓶中，加入蒸馏水，加入蒸馏水后液料比1mL:1g，然后用浓度为20％的KOH调节pH值为6.0，并向锥形瓶中填充氮气，进行第一次恒温水解，时间为30min，加入氯化钾0.5g，继续进行第二次恒温水解，时间为30min，在5000g的离心力作用下，趁热离心10min，分离出上层粗鱼油；
(2)粗鱼油的预处理：将上述步骤制取的粗鱼油加入足量乙醇和10mL浓硫酸，加热回流；将馏出物用足量的正己烷进行萃取；萃取物通过硅胶层析法，进行分离；
其中，粗鱼油进行三步真空分子蒸馏，蒸馏的真空度控制在2mmHg，温度分阶段分别截取在65-70℃、100-105℃、120-125℃三个温度段上截止轻馏分、中间馏分、重组分。
实施例2：
一种斑点叉尾鮰鱼内脏油DHA和EPA的分离纯化方法，包括以下步骤：
(1)粗鱼油的制备：处理过的斑点叉尾鮰内脏经过解冻后，放入具塞锥形瓶中，加入蒸馏水，加入蒸馏水后液料比1.5mL:1g，然后用浓度为20％的KOH调节pH值为6.5，并向锥形瓶中填充氮气，进行第一次恒温水解，时间为150min，加入氯化钾20g，继续进行第二次恒温水解，时间为160min，在5000g的离心力作用下，趁热离心10min，分离出上层粗鱼油；
(2)粗鱼油的预处理：将上述步骤制取的粗鱼油加入足量乙醇和80mL浓硫酸，加热回流；将馏出物用足量的正己烷进行萃取；萃取物通过硅胶层析法，进行分离；
其中，粗鱼油进行三步真空分子蒸馏，蒸馏的真空度控制在3mmHg，温度分阶段分别截取在65-70℃、100-105℃、120-125℃三个温度段上截止轻馏分、中间馏分、重组分。
实施例3
一种斑点叉尾鮰鱼内脏油DHA和EPA的分离纯化方法，包括以下步骤：
(1)粗鱼油的制备：处理过的斑点叉尾鮰内脏经过解冻后，放入具塞锥形瓶中，加入蒸馏水，加入蒸馏水后液料比2mL:1g，然后用浓度为20％的KOH调节pH值为7.0，并向锥形瓶中填充氮气，进行第一次恒温水解，时间为300min，加入氯化钾100g，继续进行第二次恒温水解，时间为300min，在5000g的离心力作用下，趁热离心10min，分离出上层粗鱼油；
(2)粗鱼油的预处理：将上述步骤制取的粗鱼油加入足量乙醇和200mL浓硫酸，加热回流；将馏出物用足量的正己烷进行萃取；萃取物通过硅胶层析法，进行分离；
其中，粗鱼油进行三步真空分子蒸馏，蒸馏的真空度控制在4mmHg，温度分阶段分别截取在65-70℃、100-105℃、120-125℃三个温度段上截止轻馏分、中间馏分、重组分。
最后应说明的是：以上实施例仅用以说明本发明而并非限制本发明所描述的技术方案；本领域的普通技术人员应当理解，仍然可以对本发明进行修改或等同替换；而一切不脱离本发明的精神和范围的技术方案及其改进，其均应涵盖在本发明的权利要求范围中。
Claims (10)
1.一种斑点叉尾鮰鱼内脏油DHA和EPA的分离纯化方法，其特征在于，包括以下步骤：
(1)粗鱼油的制备：处理过的斑点叉尾鮰内脏经过解冻后，放入具塞锥形瓶中，加入蒸馏水，然后用KOH调节pH值，并向锥形瓶中填充氮气，进行第一次恒温水解，加入氯化钾，继续进行第二次恒温水解，在5000g的离心力作用下，趁热离心10min，分离出上层粗鱼油；
(2)粗鱼油的预处理：将上述步骤制取的粗鱼油加入乙醇和浓硫酸，加热回流；将馏出物用足量的正己烷进行萃取；萃取物通过硅胶层析法，进行分离；
其中，粗鱼油进行三步真空分子蒸馏，温度分阶段分别截取在65-70℃、100-105℃、120-125℃三个温度段上截止轻馏分、中间馏分、重组分。
2.根据权利要求1所述的分离纯化方法，其特征在于，所述加入蒸馏水后液料比1-2mL:1g。
3.根据权利要求1所述的分离纯化方法，其特征在于，所述KOH的浓度为20％。
4.根据权利要求1所述的分离纯化方法，其特征在于，所述pH值为6.0-7.0。
5.根据权利要求1所述的分离纯化方法，其特征在于，所述第一次恒温水解的时间为30-300min。
6.根据权利要求1所述的分离纯化方法，其特征在于，所述氯化钾的加入量为0.5-100g。
7.根据权利要求1所述的分离纯化方法，其特征在于，所述乙醇为足量。
8.根据权利要求1所述的分离纯化方法，其特征在于，所述浓硫酸为10-200mL。
9.根据权利要求1所述的分离纯化方法，其特征在于，所述第二次恒温水解的时间为30-300min。
10.根据权利要求1所述的分离纯化方法，其特征在于，所述蒸馏的真空度控制在2-4mmHg。
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| CN112592268B (zh) * | 2020-12-18 | 2022-12-09 | 江苏汉邦科技股份有限公司 | 一种利用连续色谱系统分离鱼油中epa的方法 |
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