CN106497670A - Dha提取工艺 - Google Patents

Dha提取工艺 Download PDF

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CN106497670A
CN106497670A CN201610966736.3A CN201610966736A CN106497670A CN 106497670 A CN106497670 A CN 106497670A CN 201610966736 A CN201610966736 A CN 201610966736A CN 106497670 A CN106497670 A CN 106497670A
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dha
extraction
vacuum
ocean fishes
ocean
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孙明杰
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Weihai Yulong Aquatic Product Development Co Ltd
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Weihai Yulong Aquatic Product Development Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11CFATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C1/00Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
    • C11C1/02Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils
    • C11C1/04Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils by hydrolysis
    • C11C1/045Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils by hydrolysis using enzymes or microorganisms, living or dead
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11CFATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
    • C11C1/00Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
    • C11C1/08Refining

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Wood Science & Technology (AREA)
  • Microbiology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Biochemistry (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Fats And Perfumes (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

本发明提供一种DHA提取工艺,将海产品经过原料处理、脱脂脱色、酶解、真空提取、分离、浓缩、干燥等步骤,得到高活性复合DHA,本发明的优点在于,提取工艺合理有效,开创了新型海鱼提取DHA的工艺路线,极大限度地将DHA提取出来;采用酶处理和真空提取相结合的方法,DHA提取率高,反应条件温和,大大缩短了提取时间,确保提取出DHA的生物活性,使得最终产品DHA营养性与功能性兼具。

Description

DHA提取工艺
技术领域
本发明涉及的是DHA的提取技术,特别是以海鱼为原料提取DHA的技术。
背景技术
DHA,二十二碳六烯酸,俗称脑黄金,是一种对人体非常重要的多不饱和脂肪酸,属于Omega-3不饱和脂肪酸家族中的重要成员。DHA是神经系统细胞生长及维持的一种主要元素,是大脑和视网膜的重要构成成分,在人体大脑皮层中含量高达20%,在眼睛视网膜中所占比例最大,约占50%,因此,对胎婴儿智力和视力发育至关重要;DHA主要存在于海鱼中,目前DHA的提取主要是水提法和酸提法,然后采用醇沉的方法对其进行分离。这两种方法虽然简单方便,但DHA提取率低、纯度也不高,活性成分损失比较大,已经不能满足市场需求,也不适应企业发展需要。
发明内容
本发明的目的:
本发明的目的是提供一种以海鱼为原料,通过酸洗处理、粉碎、乙醇脱脂脱色、酶处理与真空提取,以及真空喷雾干燥技术,得到既能保持海鱼中粘DHA原有生物活性,又能最大限度提高DHA提取率的新工艺。
本发明的技术方案是:
一种DHA提取工艺,;
(1)原料处理:将新鲜海鱼用水洗净,沥干后,在0.05-0.1%的柠檬酸溶液中浸泡10-30min,于40-70℃烘干至含水分小于4%,再粉碎至100-200目的海鱼粉;
(2)脱脂脱色:在海鱼粉中加入10-20倍无水乙醇,60-80℃回流1-3h,4000rpm离心l0min得到混有少量乙醇的海鱼粉,于20-50℃让残留乙醇完全挥发;
(3)酶解:使用木瓜蛋白酶和纤维素酶于缓冲液中进行复合酶解:将经处理后的海鱼液用6mol/L盐酸调pH值为4-6,加入质量分数0.1-1.0%,酶活3.0×104u/g的木瓜蛋白酶和质量分数0.5-1.5%,酶活1.0×104u/g的纤维素酶,于40-60℃搅拌酶解1-2h,之后用0.5mo1/L氢氧化钠调pH至中性;
(4)真空提取:将得到的海鱼酶解液置于真空提取设备中,控制真空度85-90KPa,温度40-60℃提取1-2小时,同时灭酶,得到DHA提取液;
(5)分离:将DHA提取液于6000rpm离心20分钟,收集上清液;
(6)浓缩:将得到的DHA母液置于真空浓缩设备中,控制真空度85-90KPa,温度40-60℃浓缩至原体积的l/5-1/3,得到DHA浓缩液;
(7)干燥:将DHA浓缩液置于喷雾干燥设备中,于真空度80-120Pa,板温40-60℃,干燥10-25小时,得到高活性复合DHA。
本发明具有的优点和积极效果是:
提取工艺合理有效,开创了新型海鱼提取DHA的工艺路线,极大限度地将DHA提取出来;采用酶处理和真空提取相结合的方法,DHA提取率高,反应条件温和,大大缩短了提取时间,确保提取出DHA的生物活性,使得最终产品DHA营养性与功能性兼具;本发明采用无水乙醇回流的方法不仅将海鱼腥味的来源—高度不饱和脂肪酸去除,同时还可以去除大部分的色素,预处理过程中的酸洗也起到一定的脱腥作用;喷雾干燥技术,避免了热力干燥对DHA中活性成分的损伤。
具体实施方式
为使本发明的内容更容易被清楚地理解,下面根据具体的实施例对本发明做进一步详细的说明。
实施例1:
将1000g新鲜海鱼用水冲洗干净,沥干后,在0.1%柠檬酸溶液中浸泡30min,于40℃烘干至含水分小于4%,再粉碎至100目,得到海鱼粉226g,加入2500ml无水乙醇,60℃回流处理3h,4000rpm离心l0min得到混有少量乙醇的海鱼粉,于20℃让残留乙醇完全挥发后,加入6mol/L盐酸调pH值为4,加入质量分数0.5%,酶活3.0×104u/g的木瓜蛋白酶和质量分数1.0%,酶活1.0×104u/g的纤维素酶,于50℃搅拌酶解2h,之后用0.5mo1/L氢氧化钠调pH至中性,将得到的海鱼酶解液置于真空提取设备中,控制真空度85KPa,温度40℃提取2h,同时灭酶,得到DHA提取液于6000rpm离心20min,收集上清液,得到DHA母液,置于真空浓缩设备中,控制真空度85KPa,温度40℃浓缩至原体积的1/5,得到DHA浓缩液于喷雾干燥设备中,真空度80Pa,板温45℃,冷冻干燥25h,得到高活性复合DHA。
以上对本发明的一个实施例进行了详细说明,但所述内容仅为本发明的较佳实施例,不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的均等变化与改进等,均应仍归属于本发明的专利涵盖范围之内。

Claims (1)

1.一种DHA提取工艺,其特征在于工艺步骤为:
(1)原料处理:将新鲜海鱼用水洗净,沥干后,在0.05-0.1%的柠檬酸溶液中浸泡10-30min,于40-70℃烘干至含水分小于4%,再粉碎至100-200目的海鱼粉;
(2)脱脂脱色:在海鱼粉中加入10-20倍无水乙醇,60-80℃回流1-3h,4000rpm离心l0min得到混有少量乙醇的海鱼粉,于20-50℃让残留乙醇完全挥发;
(3)酶解:使用木瓜蛋白酶和纤维素酶于缓冲液中进行复合酶解:将经处理后的海鱼液用6mol/L盐酸调pH值为4-6,加入质量分数0.1-1.0%,酶活3.0×104u/g的木瓜蛋白酶和质量分数0.5-1.5%,酶活1.0×104u/g的纤维素酶,于40-60℃搅拌酶解1-2h,之后用0.5mo1/L氢氧化钠调pH至中性;
(4)真空提取:将得到的海鱼酶解液置于真空提取设备中,控制真空度85-90KPa,温度40-60℃提取1-2小时,同时灭酶,得到DHA提取液;
(5)分离:将DHA提取液于6000rpm离心20分钟,收集上清液;
(6)浓缩:将得到的DHA母液置于真空浓缩设备中,控制真空度85-90KPa,温度40-60℃浓缩至原体积的l/5-1/3,得到DHA浓缩液;
(7)干燥:将DHA浓缩液置于喷雾干燥设备中,于真空度80-120Pa,板温40-60℃,干燥10-25小时,得到高活性复合DHA。
CN201610966736.3A 2016-11-05 2016-11-05 Dha提取工艺 Pending CN106497670A (zh)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108185427A (zh) * 2018-02-11 2018-06-22 成都图径生物科技有限公司 含鱼眼、茶氨酸和磷脂酰丝氨酸的缓解视疲劳的组合物
WO2023043323A1 (en) * 2021-09-15 2023-03-23 Natural Extraction Technologies Limited Method of extraction from animal material, and extracts therefrom

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108185427A (zh) * 2018-02-11 2018-06-22 成都图径生物科技有限公司 含鱼眼、茶氨酸和磷脂酰丝氨酸的缓解视疲劳的组合物
WO2023043323A1 (en) * 2021-09-15 2023-03-23 Natural Extraction Technologies Limited Method of extraction from animal material, and extracts therefrom

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Application publication date: 20170315