CN104478694B - 一种从鰤鱼中提取二十二碳六烯酸和二十碳五烯酸的方法 - Google Patents
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Abstract
本发明公开了一种从鰤鱼中提取二十二碳六烯酸和二十碳五烯酸的方法，该方法是采用超临界二氧化碳流体萃取技术，通过改变夹带剂和原料比例，试验温度、压力、时间等实验条件，对富含二十二碳六烯酸和二十碳五烯酸的鰤鱼进行提取，得到这两种对人体非常重要的不饱和脂肪酸。本发明提供的提取方法萃取率高，性质稳定，具有方便、安全、环保、原料成本低等特点，适合于制备药品、保健品等，具有很高的实用意义。
Description
技术领域
本发明涉及一种从鰤鱼中提取二十二碳六烯酸和二十碳五烯酸的方法，特别涉及一种使用超临界二氧化碳流体萃取技术从鰤鱼中提取二十二碳六烯酸和二十碳五烯酸的方法。
背景技术
鰤鱼又称油甘鱼，鰤亚科、鰤属，是一种温水性鱼类，分布于日本日本海及台湾以南海域。鰤鱼含有丰富的DHA，即二十二碳六烯酸。DHA是人脑营养必不可少的高度不饱和脂肪酸。它除了能阻止胆固醇在血管壁上的沉积、预防或减轻动脉粥样硬化和冠心病的发生外，更重要的是DHA对大脑细胞有着极其重要的作用。它占了人脑脂肪的10%，对脑神经传导和突触的生长发育极为有利。实验表明，DHA摄入充分，人脑中的DHA值升高，就能活化大脑神经细胞，改善大脑功能，提高判断能力。毫无疑问，DHA具有十分显著的健脑益智作用，是青少年增进智力、加强记忆、提高学习能力的必需营养品。鰤鱼素有“补脑神品”之誉。
鰤鱼除了含有丰富的DHA，还含有另一种对人体有益的不饱和脂肪酸——EPA，即二十碳五烯酸。EPA是鱼油的主要成分。EPA属于Ω-3系列多不饱和脂肪酸，虽然亚麻酸在人体内可以转化为EPA，但此反应在人体中的速度很慢且转化量很少，远远不能满足人体对EPA的需要，因此必须从食物中直接补充。增加EPA的吸收已经证实对治疗冠状动脉心脏病、高血压和炎症（例如风湿性关节炎）有效。EPA,我们又常称血管清道夫。
经科学家研究表明，DHA和EPA只存在于鱼类及少数贝类中，其他食物如大豆、奶油、植物油、猪油、蔬菜及水果等几乎都不含有DHA。随着DHA和EPA等在药品、保健品中的广泛应用，DHA和EPA的简便高效提取显得尤为重要。鰤鱼作为一种富含DHA和EPA并且价格低廉的鱼类，很适合用来作为提取DHA和EPA的原料。本方法利用超临界二氧化碳流体萃取法，通过调节萃取压力、萃取温度、收集压力、收集温度以及夹带剂和原料的比例等，达到高效提取的效果。
发明内容
本发明提供了一种从鰤鱼中提取二十二碳六烯酸和二十碳五烯酸的方法，其原料为富含DHA和EPA的鰤鱼，通过超临界二氧化碳流体萃取工艺的萃取，得到萃取率高的鰤鱼提取物。
为了实现上述目的，本发明采用的技术方案为：利用超临界二氧化碳流体萃取法，通过调节萃取压力、萃取温度、收集压力、收集温度以及夹带剂和原料的比例等，探究不同条件下DHA和EPA的萃取效果。
一种从鰤鱼中提取二十二碳六烯酸和二十碳五烯酸的方法，按照如下步骤进行：（1）将鰤鱼进行冷冻干燥后，经粉粹，研磨后过80目筛，过筛2次，置于干燥器待用；
（2）称取50kg处理后的鰤鱼粉，上超临界二氧化碳流体萃取仪，以鰤鱼粉为原料，按照重量比，以夹带剂：鰤鱼粉=1:1~1:4的比例加入夹带剂，装釜，密封；
（3）调节萃取压力在18~30MPa的范围内，萃取温度在38~54℃之间，进行超临界二氧化碳流体萃取3小时；
（4）调节收集压力在24~36MPa的范围内，收集温度在40~60℃之间的条件下进行分离，的得到萃取物；
（5）其中，二氧化碳流量为2ml/g。
实施例中的夹带剂可以是水、甲醇、乙醇、丙酮、丙烷等，本发明实验主要用无水乙醇，其他夹带剂也可有相似效果。
本方法提取的鰤鱼提取物，其特征在于，其主要不饱和脂肪酸成分及重量百分含量为：二十二碳六烯酸30~46%，二十碳五烯酸24~40%。
本发明的有益效果是:首先，鰤鱼作为一种富含DHA和EPA并且价格低廉的鱼类，很适合用来作为提取DHA和EPA的原料。其次，本方法利用超临界二氧化碳流体萃取法，其萃取率高，性质稳定，具有方便、安全、环保、原料成本低等特点，适合于制备药品、保健品等，具有很高的实用意义。
附图说明
图1为收集压力对超临界二氧化碳流体萃取DNA和EPA的影响；
图2为萃取压力对超临界二氧化碳流体萃取DNA和EPA的影响；
图3为萃取温度对超临界二氧化碳流体萃取DNA和EPA的影响；
图4为收集温度对超临界二氧化碳流体萃取DNA和EPA的影响；
图5为夹带剂用量对超临界二氧化碳流体萃取DNA和EPA的影响。
具体实施方法
下面列举制备方面的实施例进一步详细说明本发明，该实施例仅用于本发明而对本发明并没有限制。
实施例1
（1）将鰤鱼进行冷冻干燥后，经粉粹，研磨后过80目筛，过筛2次，置于干燥器待用；
（2）称取50kg处理后的鰤鱼粉，上超临界二氧化碳流体萃取仪，以鰤鱼粉为原料，按照重量比，以夹带剂：鰤鱼粉=1:1~1:4的比例加入夹带剂，装釜，密封；
（3）调节萃取压力在18~30MPa的范围内，萃取温度在38~54℃之间，进行超临界二氧化碳流体萃取3小时；
（4）调节收集压力在24~36MPa的范围内，收集温度在40~60℃之间的条件下进行分离，的得到萃取物；
（5）其中，二氧化碳流量为2ml/g。
实施例2提取物中DHA和EPA的含量测定
本发明中实验所得的萃取物的DHA和EPA含量，依照《中华人民共和国标准》中关于“食品中二十碳五烯酸和二十二碳六烯酸的测定”（GB/T5009.168-2003）的方法进行检测。具体步骤如下：
1.样品溶液的制备：
（1）皂化：取实施例1中的萃取物1g于50ml具塞容量瓶中，加入10ml正己烷轻摇使油脂融解，并用正己烷定容至刻度。吸取此处溶液3.00ml于另一具塞比色管中，再加入2ml/L氢氧化钠-甲醇溶液1ml，充分振荡10min后放入60℃的水浴中加热1min~2min，皂化完成后，冷却至室温，带甲酯化用；
（2）甲酯化：加入2mol/L盐酸-甲醇溶液2ml，充分振荡10min，并于50℃的水浴中加热2min，进行甲酯化，弃去下层液体，再加约2ml蒸馏水洗净并去除水层，用滴管吸出正己烷层，移到另一装有无水硫酸钠的漏斗中脱水，将脱水后的溶液在70℃水浴上加热浓缩，定容至1ml，带上机测试。
2.标准液的配制：
将EPA甲酯和DHA甲酯标准品用正己烷配制成浓度依次为0.5、1.0、2.5mg/ml的标准液。
3.气相色谱的条件：
采用GC-2010色谱分析仪，DB-23毛细管色谱柱（60m*0.250mm*0.25μm）。进样口温度为250℃；FID检测温度为280℃；载气为高纯度氦气，230Kpa恒压（或33cm/s，50℃时）；非线性程序升温：50℃保持1min后，以25℃/min的速度升至175℃，再以5℃/min升至230℃保持13min；进样体积为1μL，分流比50：1。
4.检测结果：见附图1~5。
Claims (2)
1.一种从鰤鱼中提取二十二碳六烯酸和二十碳五烯酸的方法，其特征在于，按照如下步骤进行：
（1）将鰤鱼进行冷冻干燥后，经粉粹，研磨后过80目筛，过筛2次，置于干燥器待用；
（2）称取50kg处理后的鰤鱼粉，上超临界二氧化碳流体萃取仪，以鰤鱼粉为原料，按照重量比，以夹带剂：鰤鱼粉=1:1~1:4的比例加入夹带剂，装釜，密封；
（3）调节萃取压力在18~30MPa的范围内，萃取温度在38~54℃之间，进行超临界二氧化碳流体萃取3小时；
（4）调节收集压力在24~36MPa的范围内，收集温度在40~60℃之间的条件下进行分离，得到萃取物；
（5）其中，二氧化碳流量为2ml/g，
上述夹带剂选自水、甲醇、乙醇、丙酮。
2.一种从鰤鱼中提取二十二碳六烯酸和二十碳五烯酸的方法，其特征在于，按照如下步骤进行：
（1）将鰤鱼进行冷冻干燥后，经粉粹，研磨后过80目筛，过筛2次，置于干燥器待用；
（2）称取一定量处理后的鰤鱼粉，上超临界二氧化碳流体萃取仪，以鰤鱼粉为原料，按照重量比，以夹带剂：鰤鱼粉=1:4的比例加入夹带剂，装釜，密封；
（3）调节萃取压力在22MPa，萃取温度在50℃，进行超临界二氧化碳流体萃取3小时；
（4）调节收集压力在32MPa，收集温度在55℃的条件下进行分离，得到萃取物；
（5）其中，二氧化碳流量为2ml/g，
上述夹带剂选自水、甲醇、乙醇、丙酮。
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