CN102429215A - Linolenic acid microcapsules and preparation method thereof - Google Patents

Linolenic acid microcapsules and preparation method thereof Download PDF

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CN102429215A
CN102429215A CN 201110323849 CN201110323849A CN102429215A CN 102429215 A CN102429215 A CN 102429215A CN 201110323849 CN201110323849 CN 201110323849 CN 201110323849 A CN201110323849 A CN 201110323849A CN 102429215 A CN102429215 A CN 102429215A
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linolenic acid
microcapsules
purity
prepared
gum
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CN 201110323849
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CN102429215B (en )
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刘霞
张炜
徐江波
池亚玲
王平平
肖江
范燕青
蔡林森
赵文华
郭幼敬
郭智军
陈元涛
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陈元涛
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Abstract

The invention relates to linolenic acid microcapsules and a preparation method thereof. The preparation method comprises the following steps of: adopting the linseed oil as the raw material to prepare the linolenic acid of which the purity is 70-90%; uniformly mixing the linolenic acid of which the purity is 70-90%, linseed gum and water, and heating to 50-60 DEG C; homogenizing at 30-40 MPa for 30 min to obtain the emulsion liquid; finally atomizing and drying the emulsion liquid to prepare the microcapsules. The linolenic acid microcapsules prepared by the invention has the advantages that the microcapsules have long shelf-life and high oil content rate which is up to 60%. The linolenic acid microcapsules adopt the high-pure linolenic acid, so the active component Alpha-linolenic acid of the microcapsules in unit mass is increased for two times; the linolenic acid microcapsules and the preparation method thereof switch the linseed oil into the linolenic acid, the water solubility ofthe linolenic acid is improved, and the compatibility between the linolenic acid and the linseed gum is improved, so the emulsification before atomizing and drying can be smoothly implemented, the emulsifying agent does not need to use, and the edible safety of the microcapsules can be ensured; and the linolenic acid microcapsules and the preparation method thereof adopt the linseed gum as the wall material of the microcapsules, so that the use of the linseed gum is enlarged.

Description

一种亚麻酸微胶囊及其制备方法 One kind of linolenic acid and preparation method of microcapsules

技术领域 FIELD

[0001] 本发明涉及一种胶囊及其制备方法,尤其涉及一种亚麻酸微胶囊及其制备方法。 [0001] The present invention relates to a capsule preparation method thereof, and particularly to micro-linolenic acid and a capsule preparation method. 背景技术 Background technique

[0002] 亚麻为亚麻科、亚麻属一年生或多年生草本植物,是我国主要经济作物之一,也是我国华北、西北高寒地区的主要油料作物。 [0002] flax to linen families, flax is an annual or perennial herb, is one of the major cash crops, is also a major oil crops in North China, Northwest alpine region. 亚麻籽是亚麻的种子,含有脂肪、蛋白质、可食纤维和黏胶等成分。 Linseed flax seeds, containing fat, protein, dietary fibers and viscose and other ingredients. 亚麻籽油,又称亚麻油,是从亚麻籽中制取的油,含45〜53% α-亚麻酸,19〜四%油酸,14〜18%亚油酸,9〜11%饱和脂肪酸。 Linseed oil, also known as linseed oil, from flaxseed oil preparation containing 45~53% α- linolenic acid, 19~ four percent oleic acid, linoleic acid 14~18%, 9~11% saturated fatty acids .

[0003] 众所周知,α-亚麻酸是世界公认的人体必需脂肪酸,人体不能自身合成,只能从食品中摄取。 [0003] As we all know, α- linolenic acid is recognized worldwide as essential fatty acids, the body can not synthesize their own, only intake from food. 国内外大量的科学研究表明α-亚麻酸在改善人类营养结构与增强健康等方面具有非常重要的应用价值,如发现α -亚麻酸对婴幼儿脑部发育,调节免疫系统,降血脂、降低血液粘稠度和抑制恶性肿瘤等方面均有一定功效。 A large number of domestic and foreign scientific research shows that α- linolenic acid has a very important value in human nutrition structure and enhance the health and other aspects, such as found in α - linolenic acid on infant brain development, regulation of the immune system, lowering blood pressure, reduce blood consistency and aspect to suppress malignant tumors have a certain effect. 由于α-亚麻酸在生产加工、贮藏和烹饪等过程中易氧化变质,产生难闻的腥臭味,这不仅影响其食用安全,还影响它的普及与推广,进而最终严重影响其营养和保健功能的发挥。 Because of α- linolenic acid is easy to oxidative deterioration in the production, processing, storage and cooking process, resulting in an unpleasant fishy smell, which affects not only their food safety, but also affected its popularity and promotion, and then ultimately seriously affect their nutrition and health care functions play. 另外,液态α-亚麻酸也很难添加至日常食品(如面条、面包)中,使人们对其摄取成为一大难题。 In addition, liquid α- linolenic acid is also difficult to add to the daily food (such as pasta, bread), the uptake of its people has become a major problem.

[0004] 微胶囊是指由天然或人工合成的高分子材料制成的具有聚合物壁壳的微型容器或包装物。 [0004] The microcapsules refers to a polymer having a micro-container wall or shell wrapper from a natural or synthetic polymer material. 微胶囊技术可以改变物质形态、保护敏感成分、隔离活性物质和降低挥发性等。 Microencapsulation can change the physical form, to protect sensitive ingredients, isolation and reduce the volatility of the active material and the like. 近年来,微胶囊技术在高附加值油脂产品制备领域中是令人关注的热点之一。 In recent years, microencapsulation technology is the focus of concern in the manufacture of high value-added oil products in the field.

[0005] 在研究中发现,已有很多文献提及亚麻酸相关的微胶囊技术,但是现有技术都是以明胶、阿拉伯胶和改性淀粉等为壁材制取微胶囊,生产过程中需要用到大量的合成乳化剂,会影响微胶囊食用安全,另外,现有的微胶囊壁材包封不好,致使壁材使用量大,如文献通常报道的微胶囊含油率小于40%,单位质量的微胶囊中亚麻酸含量不足18%。 [0005] In the study found a lot of literature already mentioned linolenic related microencapsulation, but the prior art are gelatin, gum arabic and modified starch as the preparation of the microcapsule wall material, the production process requires use a lot of synthetic emulsifier, microcapsules can affect food safety, further, the conventional encapsulating microcapsule wall material is not good, resulting in a large amount using a wall material, microcapsule oil content is generally reported in the literature is less than 40%, the unit mass microcapsules linolenic acid content is less than 18%.

发明内容 SUMMARY

[0006] 本发明针对现有亚麻酸微胶囊存在的上述不足,提供一种亚麻酸微胶囊及其制备方法。 [0006] The present invention addresses the above shortcomings of the prior microcapsules linolenic acid, linolenic acid, and to provide one kind of the microcapsules preparation.

[0007] 本发明解决上述技术问题的技术方案如下:一种亚麻酸微胶囊的制备方法包括以下步骤: [0007] solve the above problems of the present invention, the following technical solution: A method for preparing microcapsules linolenic acid comprises the steps of:

[0008] 步骤一:采用亚麻油为原料制备纯度为70〜90%的亚麻酸; [0008] Step 1: The starting material for the linseed oil is prepared in a purity of 70~90% linolenic acid;

[0009] 步骤二:将纯度为70〜90%的亚麻酸、亚麻胶和水混合均勻,升温至50〜60°C, 在压力30〜40MPa下高压均质30分钟制成稳定乳液,其中,所述亚麻酸和亚麻胶的质量比不超过3 : 2,所述水的质量为亚麻胶和亚麻酸混合物质量的6〜10倍; [0009] Step 2: 70~90% purity linolenic acid flax gum and water were mixed uniformly, warmed to 50~60 ° C, 30 minutes to prepare a stable emulsion in a high pressure homogenizer at a pressure 30~40MPa, wherein the quality and linolenic acid flax gum is no more than 3: 2, the quality of the water and gum mixture 6~10 times the mass of the flax linolenic acid;

[0010] 步骤三:将乳液进行喷雾干燥后制备微胶囊,干燥参数是:进料温度为50〜60°C, 进风温度为170〜230°C,出风温度为70〜90°C。 [0010] Step 3: Preparation of emulsion microcapsules after spray drying, drying parameters: feed temperature is 50~60 ° C, inlet air temperature is 170~230 ° C, the air temperature is 70~90 ° C.

[0011] 在上述技术方案的基础上,本发明还可以做如下改进。 [0011] Based on the foregoing technical solution, the present invention may be modified as follows.

[0012] 进一步,当步骤一采用尿素包合法制备纯度为70〜90%的亚麻酸时,其具体的工艺条件是:将亚麻油和lmol/L KOH-EtOH溶液按质量比为1 : 4混合,在60°C水浴中搅拌1〜2小时至完全皂化,加入稀盐酸调节pH至1〜1. 5,用正己烷萃取2次,合并上层油状液体,用水洗至中性,回收正己烷,即得混合脂肪酸;将混合脂肪酸、尿素和乙醇按质量比1:3: 5依次加入到反应容器里,在75°C下搅拌1小时后,于-15°C静置12小时,过滤除去结晶;滤液再次加入尿素,重复搅拌、静置和过滤等操作1〜3次,回收乙醇,即得高纯亚麻酸。 [0012] Further, when the step of using a urea adduction prepared purity of 70~90% linolenic acid, and specific process conditions are: the linseed oil and lmol / L KOH-EtOH solution a mass ratio of 1: 4 mixed the mixture was stirred at 60 ° C water bath for 1 to 2 hours to complete saponification, dilute hydrochloric acid was added to adjust the pH to 1~1. 5, extracted twice with n-hexane, the upper oily liquid were combined, washed with water until neutral, n-hexane recovery, i.e., obtain a mixed fatty acid; the mixed fatty acid, ethanol, and urea mass ratio of 1: 3: 5 was successively added to the reaction vessel, stirring at 75 ° C 1 h, allowed to stand for 12 hours at -15 ° C, crystals removed by filtration ; urea filtrate was added again repeated stirring, settling and filtration operations 1~3 times, recovery of ethanol, to obtain high purity linolenic acid. 值得强调的是,为了使高纯度α-亚麻酸更加稳定,也可以进一步制成亚麻酸乙酯或亚麻酸甲酯等。 It is worth emphasizing that, in order to make more stable high-purity α- linolenic acid, it may further be made of linen or linen, ethyl and methyl.

[0013] 进一步,当步骤一采用分子蒸馏法制备纯度为70〜90%的亚麻酸时,其具体的工艺条件是:蒸馏压力0. 2〜0. 3Pa,蒸馏温度120°C,刮膜转速200r/min,蒸馏2〜4次。 [0013] Further, when a step was prepared by molecular distillation method and a purity of 70~90% linolenic acid, and specific process conditions are: distillation pressure 0. 2~0 3Pa, a distillation temperature of 120 ° C, wiper speed of film 200r / min, distillation ~ 4 times.

[0014] 在喷雾过程中,进风与出风温度是产品质量的重要因素。 [0014] In the spraying process, the air inlet and outlet temperature is an important factor in the quality of products. 太高的温度会使微胶囊的外部壁材产生裂痕,影响包囊的效果。 Too high a temperature will external wall material of the microcapsule cracks, influence the effect of encapsulation. 温度太低产品的水分含量高,产品不宜保持。 High temperature is too low moisture content of the product, the product should not be maintained.

[0015] 本发明的有益效果是:本发明以高纯亚麻酸为内包物,以加工亚麻油所得副产品亚麻胶为壁材,模拟亚麻籽的天然存在形态来制备亚麻酸微胶囊,制备的亚麻酸微胶囊具有易保存、微胶囊含油率最高达60%的优点;选用高纯亚麻酸,从而使单位质量的微胶囊中亚麻酸含量提高近两倍;将亚麻油转换成亚麻酸,可避免喷雾干燥前乳化剂的使用,以保证食用安全;同时拓展了亚麻胶的用途。 [0015] Advantageous effects of the present invention are: the present invention is encapsulated in a high purity linolenic acid was obtained in a linseed oil-products processing flax gum as wall materials, the microcapsules prepared linolenic acid analog of the naturally occurring form of linseed, flax prepared acid microcapsules have the advantage of easy to preserve maximum oil content of the microcapsules was 60%; the choice of high purity linolenic acid, so that the mass per unit microcapsules linolenic acid content increased almost twice; converting into linolenic acid linseed oil, can be avoided emulsifiers spray dried before use, in order to ensure food security; at the same time expanding the use of flax glue.

具体实施方式 detailed description

[0016] 以下对本发明的原理和特征进行描述,所举实例只用于解释本发明,并非用于限定本发明的范围。 [0016] hereinafter be described principles and features of the present invention, The examples only serve to explain the present invention and are not intended to limit the scope of the invention.

[0017] 亚麻胶是以亚麻籽为原料,从亚麻籽壳皮中提取而得,亚麻胶是一种以多糖为主, 含有少量蛋白质的天然高分子植物胶,具有粘度高、乳化性强、保湿性和悬浮稳定性突出等特点,食用安全,目前是国际上正在发展的胶种之一,且是在加工亚麻籽的过程中得到的辅料,在节省资源的同时提高了产品的质量。 [0017] The flax is flaxseed gum as a raw material, the extract obtained from flax seed husk, flax-based gum is a polysaccharide, a natural polymer containing a small amount of protein is vegetable gum, having a high viscosity, emulsifiability and strong, moisturizing and suspension outstanding stability characteristics, food safety, is now one of the world types of plastic are being developed, and are obtained during the processing of flaxseed in materials, while saving resources, improving the quality of the product. 用亚麻胶包合亚麻酸是模仿了亚麻籽的天然存在形态,能够更好的保存内包物的营养成分。 Linolenic acid flax gum inclusion is a naturally occurring form mimics the flaxseed, more nutrients can be stored within the package thereof.

[0018] 实施例1 [0018] Example 1

[0019] 首先,采用亚麻油为原料,尿素包合法制备纯度为70%的亚麻酸;接着,将纯度为70%的亚麻酸、亚麻胶和水以质量比2 : 3 : 30混合后在30MPa进行高压均质处理30分钟后;最后,将经高压均质处理后的亚麻胶和亚麻酸的混合物以温度50°C进料,进风温度为170°C,出风温度为70°C条件下进行喷雾干燥后制备微胶囊。 [0019] First, as raw linseed oil, urea adduction prepared linolenic acid of 70% purity; Next, 70% purity linolenic acid flax gum and water at a mass ratio 2: 3: 30 mixing 30MPa high pressure homogenization for 30 minutes; finally, the mixture was homogenized by high-pressure flax gum after linolenic acid and at a temperature of 50 ° C feed, inlet air temperature of 170 ° C, air temperature of 70 ° C condition for the preparation of microcapsules after spray drying.

[0020] 经过实施例1制备的亚麻酸微胶囊的含油率为40%,单位质量的微胶囊亚麻酸为28%。 [0020] After linolenic acid oil microcapsules prepared according to Example 1 was 40%, linolenic acid per unit mass of the microcapsule was 28%.

[0021] 实施例2 [0021] Example 2

[0022] 首先,采用亚麻油为原料尿素包合法制备纯度为90%的亚麻酸;接着,将纯度为90%的亚麻酸、亚麻胶和水以质量比3 : 2 : 50混合后在40MPa进行高压均质处理;最后, 将经高压均质处理后的亚麻胶和亚麻酸的混合物以温度60°C进料,进风温度为230°C,出风温度为90°C条件下进行喷雾干燥后制备微胶囊。 [0022] First, as raw linseed oil by urea adduction prepared purity of 90% linolenic acid; then, the purity of 90% linolenic acid, flax gum and water at a mass ratio 3: 40MPa performed after mixing 50: 2 high pressure homogenization; Finally, the mixture was homogenized by high-pressure flax gum after linolenic acid and at a temperature of 60 ° C feed, inlet air temperature of 230 ° C, the air temperature was 90 ° C for spray drying conditions after the preparation of microcapsules.

[0023] 经过实施例2制备的亚麻酸微胶囊的含油率为60%,单位质量的微胶囊亚麻酸含量为54%。 [0023] After linolenic acid oil microcapsules prepared in Example 2 was 60% embodiment, the microcapsules linolenic acid content per unit mass of 54%. [0024] 实施例3 [0024] Example 3

[0025] 首先,采用亚麻油为原料分子蒸馏制备纯度为80%的亚麻酸;接着,将亚麻胶、纯度为80%的亚麻酸和水以质量比1 : 1 : 16混合后在35MPa进行高压均质处理;最后,将经高压均质处理后的亚麻胶和亚麻酸的混合物以55°C进料,进风温度为210°C,出风温度为80°C条件下进行喷雾干燥后制备微胶囊。 [0025] First, as raw linseed oil prepared molecular distillation to a purity of 80% linolenic acid; Next, flax gum, a purity of 80% linolenic acid and water at a mass ratio of 1: 16 after the high pressure at 35MPa mixing: 1 homogenization; Finally, the mixture was homogenized by high-pressure flax gum and the linolenic acid feed to 55 ° C, inlet air temperature of 210 ° C, the air temperature is prepared in the spray-dried condition of 80 ° C for Microcapsules.

[0026] 经过实施例3制备的亚麻酸微胶囊的含油率为50%,单位质量的微胶囊亚麻酸含量为40%。 [0026] After linolenic acid oil microcapsules prepared in Example 3 of the embodiment was 50%, per unit mass of the microcapsules linolenic acid content is 40%.

[0027] 以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。 [0027] The foregoing is only preferred embodiments of the present invention, not intended to limit the present invention within the spirit and principle of the present invention, any modification, equivalent replacement, or improvement, it should be included in the present within the scope of the invention.

Claims (5)

  1. 1. 一种亚麻酸微胶囊的制备方法,其特征在于,所述制备方法包括以下步骤:步骤一:采用亚麻油为原料制备纯度为70〜90%的亚麻酸;步骤二:将纯度为70〜90%的亚麻酸、亚麻胶和水混勻并升温至50〜60°C,在压力30〜40MI^下高压均质30分钟制成乳液,其中,所述亚麻酸和亚麻胶的质量比最高为3 : 2,所述水的质量为亚麻胶和亚麻酸混合物质量的6〜10倍;步骤三:将乳液进行喷雾干燥后制备微胶囊。 1. A method for preparing microcapsules linolenic acid, wherein the preparation method comprises the following steps: Step 1: The starting material for the linseed oil is prepared in a purity of 70~90% linolenic; Step 2: purity of 70 ~ 90% of linolenic acid, flax gum and water mixed and heated to 50~60 ° C, 30 minutes to prepare an emulsion in a high pressure homogenizer under pressure 30~40MI ^ mass wherein the ratio of gum linolenic acid flax and up to 3: 2, the mass of water is 6~10 times flax quality gum and a mixture of linolenic acid; step 3: preparation of emulsion microcapsules after spray drying.
  2. 2.根据权利要求1所述亚麻酸微胶囊的制备方法,其特征在于,当步骤一采用尿素包合法制备纯度为70〜90%的亚麻酸时,其具体的工艺条件是:将亚麻油和lmol/L KOH-EtOH溶液按质量比为1 : 4混合,在60°C水浴中搅拌1〜2小时至完全皂化,加入稀盐酸调节PH至1〜1.5,用正己烷萃取2次,合并上层油状液体,用水洗至中性,回收正己烷,即得混合脂肪酸;将混合脂肪酸、尿素和乙醇按质量比1 : 3 : 5依次加入到反应容器, 在75°C下搅拌1小时后,于_15°C静置12小时,过滤除去结晶;滤液再次加入尿素,重复搅拌、静置和过滤等操作1〜3次,回收乙醇,即得高纯亚麻酸。 2. The method of claim 1 prepared linolenic acid microcapsules as claimed in claim, wherein, when the step of using a urea adduction prepared purity of 70~90% linolenic acid, and specific process conditions are: the linseed oil and lmol / L KOH-EtOH solution a mass ratio of 1: 4 were mixed and stirred at 60 ° C water bath for 1 to 2 hours to complete saponification, dilute hydrochloric acid was added to adjust the PH ~ 1.5, extracted twice with n-hexane and the combined upper layer oily liquid, washed with water until neutral, recovery hexane, to give the mixed fatty acid; the mixed fatty acid, ethanol, and urea mass ratio of 1: 3: 5 were added to the reaction vessel, stirred at 75 ° C 1 hour in _15 ° C stand for 12 hours, crystals removed by filtration; the filtrate was added urea again repeated stirring, settling and filtration operations 1~3 times, recovery of ethanol, to obtain high purity linolenic acid.
  3. 3.根据权利要求1所述亚麻酸微胶囊的制备方法,其特征在于,当步骤一采用分子蒸馏法制备纯度为70〜90%的亚麻酸时,其具体的工艺条件是:蒸馏压力0. 2〜0. 3Pa,蒸馏温度120°C,刮膜转速200r/min,蒸馏2〜4次。 3. The method of claim 1 prepared linolenic acid microcapsules as claimed in claim, characterized in that, when prepared using a molecular distillation step Method purity of 70~90% of linolenic acid, the specific process conditions were: 0 distillation pressure. 2~0. 3Pa, a distillation temperature of 120 ° C, wiped film speed 200r / min, distillation ~ 4 times.
  4. 4.根据权利要求1所述亚麻酸微胶囊的制备方法,其特征在于,所述步骤二中首先使亚麻胶分散于50〜60°C的水中,再加入纯度为70〜90%的亚麻酸混合均勻。 4. The method of claim 1 prepared linolenic acid microcapsules as claimed in claim wherein said step II is first dispersed in water in flax gum 50~60 ° C, and then added with a purity of 70~90% linolenic acid well mixed.
  5. 5.根据权利要求1所述亚麻酸微胶囊的制备方法,其特征在于,所述步骤三中喷雾干燥的进料温度为50〜60°C,进风温度为170〜230°C,出风温度为70〜90°C。 5. The method of claim 1 prepared linolenic acid microcapsules as claimed in claim wherein said step of spray drying the temperature of the three feed for 50~60 ° C, inlet air temperature is 170~230 ° C, wind temperature of 70~90 ° C.
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CN103461988B (en) * 2013-07-29 2015-05-13 河北欣奇典生物科技有限公司 High-content alpha-linolenic acid microcapsule and manufacturing method thereof

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