CN1222278C - Alpha-linolenic acid microcapsule and its preparing process - Google Patents
Alpha-linolenic acid microcapsule and its preparing process Download PDFInfo
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- CN1222278C CN1222278C CN 01112968 CN01112968A CN1222278C CN 1222278 C CN1222278 C CN 1222278C CN 01112968 CN01112968 CN 01112968 CN 01112968 A CN01112968 A CN 01112968A CN 1222278 C CN1222278 C CN 1222278C
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- Prior art keywords
- linolenic acid
- alpha
- weight
- wall material
- microcapsule
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 title claims abstract description 63
- 235000020661 alpha-linolenic acid Nutrition 0.000 title claims abstract description 38
- 229960004488 linolenic acid Drugs 0.000 title claims abstract description 38
- 239000003094 microcapsule Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims description 14
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000000605 extraction Methods 0.000 claims abstract description 22
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229920002774 Maltodextrin Polymers 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000005913 Maltodextrin Substances 0.000 claims abstract description 8
- 235000010489 acacia gum Nutrition 0.000 claims abstract description 8
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims abstract description 8
- 229940035034 maltodextrin Drugs 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000001694 spray drying Methods 0.000 claims abstract description 6
- 230000001476 alcoholic effect Effects 0.000 claims description 12
- 239000010779 crude oil Substances 0.000 claims description 12
- 229920000881 Modified starch Polymers 0.000 claims description 10
- 230000001804 emulsifying effect Effects 0.000 claims description 10
- 235000019426 modified starch Nutrition 0.000 claims description 10
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 claims description 7
- 239000004368 Modified starch Substances 0.000 claims description 7
- 238000004508 fractional distillation Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000839 emulsion Substances 0.000 claims description 5
- 229920002521 macromolecule Polymers 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 125000005481 linolenic acid group Chemical group 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- 238000004945 emulsification Methods 0.000 abstract description 2
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 abstract 1
- 239000001341 hydroxy propyl starch Substances 0.000 abstract 1
- 235000013828 hydroxypropyl starch Nutrition 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 239000000084 colloidal system Substances 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 230000005070 ripening Effects 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- -1 fatty acid ester Chemical class 0.000 description 1
- 235000021323 fish oil Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000199 molecular distillation Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 210000004681 ovum Anatomy 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 239000006188 syrup Substances 0.000 description 1
- 235000020357 syrup Nutrition 0.000 description 1
Abstract
The present invention relates to an alpha-linolenic acid microcapsule and a manufacturing method thereof. The wall materials of the microcapsule are composed of 1 part of arabic gum, 1 to 1.5 parts of maltodextrin and 3 to 10 parts of hydroxypropyl starch. The manufacturing method comprises the steps that the wall materials are prepared, and supercritical CO2 is used for extracting alpha-linolenic acid; monostearin is added for emulsification, and the mixture is stirred and granulated by spray drying; the extraction pressure is from 30 to 60Mpa, the extraction temperature is from 40 to 50 DEG C., and the use concentration of an ethanol solution as entrainer is from 75 to 95 %; powdered microcapsule particles are manufactured to be isolated from air, and the linolenic acid is not easy to oxidate; the water content is less than or equal to 1.25%, the dissolvability is more than or equal to 98%, and the content of the linolenic acid can not be changed after the linolenic acid is placed for a plurality of months. Components in the wall materials are suitable for various people, the extraction rate is raised by an extraction method, and the present invention has the advantages of high concentration of the linolenic acid and simple treatment of residues.
Description
The invention provides the alpha-linolenic acid microcapsule and the manufacture method thereof of from Caulis et Folium Lini crude oil or Semen Lini, purifying and making.
Alpha-linolenic acid is a kind of easy oxidation, is difficult for preserving, should not directly adding the nutrient substance of food that it is only adopting microcapsule formulations.Make the technical problem that microcapsule generally will solve two aspects, one is the wall material formula, and a core is purified, and does not also have the wall material formula and the core method of purification of ready-made suitable manufacturing alpha-linolenic acid microcapsule at present, so, do not see the alpha-linolenic acid microcapsule listing.Technology related to the present invention has: have research institution to propose the conception of fish oil micro-capsule, use Ovum Gallus domesticus album and syrup to make the wall material, advantage is a good film-forming property, and shortcoming is the cost height, and some crowd should not take as diabetics; The report supercritical CO is arranged
2Extract linolenic from oleum lini: (1) carries out supercritical extraction to oleum lini, extractant is a liquid CO 2, the addition volume ratio is: carbon dioxide: oleum lini=2～4: 1, pressure is 150～250 atmospheric pressure, extraction temperature is 25～90 ℃, dispersant is the bead of diameter 0.5～3mm, and the addition of dispersant is 5～20WT%, and the extraction time is 0.5～2 hour; (2) above-mentioned extract is carried out decompression separation, carbon dioxide is removed, obtain first phase linolenic acid, the decompression separation time is 0.5～1 hour; (3) first phase linolenic acid is carried out rectification, rectificating method is post rectification or molecular distillation, obtains the high-purity linolenic acid.This method extraction yield is low, residual post processing complexity.
The purpose of this invention is to provide a kind of alpha-linolenic acid microcapsule, select to have high dissolution and good emulsification property, drying property, low viscous wall material so that and oleum lini be complementary and make high-quality stable and diffluent Powdered microcapsule.
Another purpose of the present invention provides the method that from oleum lini or Semen Lini purification linolenic acid is made this alpha-linolenic acid microcapsule.
Technical scheme of the present invention is:
A kind of alpha-linolenic acid microcapsule comprises linolenic acid core and wall material, it is characterized in that the wall material is made up of arabic gum, maltodextrin and modified starch, and its weight ratio is: arabic gum 1, maltodextrin 1-1.5, modified starch 3-10.
A kind of method of making above-mentioned alpha-linolenic acid microcapsule is characterized in that comprising the steps:
Preparation wall material:
(1) with 1 part of arabic gum (weight ratio, down together), maltodextrin 1-1.5 part is dissolved in hot water, and 50～70 ℃ of water temperatures are made viscosity 30-40Mpa.s water-soluble macromolecule pastel;
(2) modified starch 3-10 part is added above-mentioned pastel, mix, homogenizing, standby;
Preparation alpha-linolenic acid core:
(1) with oleum lini crude oil or Semen Lini supercritical CO
2The extraction alpha-linolenic acid, extracting pressure 30～60Mpa, 40～50 ℃ of extraction temperature, the entrainer working concentration is 75～95% alcoholic solution, the addition of alcoholic solution is 5～60% of oleum lini crude oil or a Semen Lini weight;
(2) above-mentioned extract being made linolenic acid purity with the rectifying column fractional distillation is 60～90% oleum lini;
(3) oleum lini that above-mentioned fractional distillation is made adds monoglyceride emulsifying, and it is standby to make core, and the addition of monoglyceride is 0.5～1.2% of an oleum lini weight, 60～70 ℃ of emulsifying temperatures, emulsion rotary viscosity 35-40MPaS;
With the core of preparation and wall material by weight 15-30: 100 preparations mix, and stir, and spray-drying process, dry wind advance machine 170-200 ℃, out-of-machine temperature 60-80 ℃, after the cooling alpha-linolenic acid microcapsule.
In the wall material raw material of the present invention, arabic gum, maltodextrin constitute macromolecular network, and modified starch is filled and wherein formed fine and close micel, is wrapped in oleum lini microdroplet outside, forms the microcapsule granule of powder-like, has completely cut off air, and linolenic acid is difficult for oxidized; Microcapsule moisture≤1.25% of making, dissolubility 〉=98%; After placing the several months, linolenic content is constant; Composition in the wall material is applicable to various crowds.Extracting process of the present invention is clear and definite technological parameter: extracting pressure 30～60Mpa, pressure are lower than 30Mpa and can't extract, and it is big to be higher than 60Mpa pressure, and equipment investment expense height, operating cost are big; The entrainer working concentration is 75～95% alcoholic solution, and extraction temperature can be controlled in 40～50 ℃, and the addition of alcoholic solution is 5～60% of oleum lini crude oil or a Semen Lini weight; The fatty acid ester that ethanol and oleum lini form has improved oleum lini at CO
2In dissolubility; Such extracting process has improved extraction yield, selects for use ethanol as entrainer, and the linolenic concentration height of gained can reach more than 80%, and residual post processing is simple.
Provide embodiments of the invention below and be further described.
Embodiment one:
System wall material: 3 kilograms of arabic gums add 10 kilograms of 50～70 ℃ of hot water, and (temperature is lower than 50 ℃ and is difficult for dissolving, temperature is higher than 70 ℃, and easily ripening is agglomerating water insoluble) after the dissolving, add 3 kilograms of maltodextrins again, fully stirring and evenly mixing is made viscosity 30Mpa.s water-soluble macromolecule pastel; Add 9 kilograms of modified starches to pastel again under the constant temperature, micropowder in colloid mill (degrees of detail 70 μ m) mixes, and homogenizing is standby;
Coremaking material: with oleum lini crude oil or Semen Lini supercritical CO
2The extraction alpha-linolenic acid, extracting pressure 30Mpa, 40 ℃ of extraction temperature, the entrainer working concentration is 75% alcoholic solution, the addition of alcoholic solution is 5% of oleum lini crude oil or a Semen Lini weight;
It is 60% oleum lini that above-mentioned extract is made linolenic acid purity with the rectifying column fractional distillation;
Get above-mentioned CO
23.75 kilograms of the oleum linis of extraction add 22 gram monoglyceride emulsifyings, 60 ℃ of emulsifying temperatures, the emulsion of rotary viscosity 35MPaS, standby;
Above-mentioned core and wall material are mixed, and through homogenizer (or colloid mill) homogenizing, spray-drying process, dry wind advance machine 170-200 ℃, out-of-machine temperature 60-80 ℃, get alpha-linolenic acid microcapsule after the cooling.
Embodiment two:
System wall material: 3 kilograms of arabic gums add 10 kilograms of 50～70 ℃ of hot water, and (temperature is lower than 50 ℃ and is difficult for dissolving, temperature is higher than 70 ℃, and easily ripening is agglomerating water insoluble) after the dissolving, add 4.5 kilograms of maltodextrins again, fully stirring and evenly mixing is made viscosity 40Mpa.s water-soluble macromolecule pastel; Add 30 kilograms of modified starches to pastel again under the constant temperature, micropowder in colloid mill (degrees of detail 70 μ m) mixes, and homogenizing is standby;
Coremaking material: with oleum lini crude oil or Semen Lini supercritical CO
2The extraction alpha-linolenic acid, extracting pressure 60Mpa, 50 ℃ of extraction temperature, the entrainer working concentration is 95% alcoholic solution, the addition of alcoholic solution is 60% of oleum lini crude oil or a Semen Lini weight;
It is 90% oleum lini that above-mentioned extract is made linolenic acid purity with the rectifying column fractional distillation;
Get above-mentioned CO
214.25 kilograms of the oleum linis of extraction add 170 gram monoglyceride emulsifyings, 70 ℃ of emulsifying temperatures, the emulsion of rotary viscosity 40MPaS, standby;
Above-mentioned core and wall material are mixed, and through homogenizer (or colloid mill) homogenizing, spray-drying process, dry wind advance machine 170-200 ℃, out-of-machine temperature 60-80 ℃, get alpha-linolenic acid microcapsule after the cooling.
Embodiment three:
System wall material: 3 kilograms of arabic gums add 10 kilograms of 50～70 ℃ of hot water, and (temperature is lower than 50 ℃ and is difficult for dissolving, temperature is higher than 70 ℃, and easily ripening is agglomerating water insoluble) after the dissolving, add 3.6 kilograms of maltodextrins again, fully stirring and evenly mixing is made viscosity 35Mpa.s water-soluble macromolecule pastel; Add 20 kilograms of modified starches to pastel again under the constant temperature, micropowder in colloid mill (degrees of detail 70 μ m) mixes, and homogenizing is standby;
Coremaking material: with oleum lini crude oil or Semen Lini supercritical CO
2The extraction alpha-linolenic acid, extracting pressure 45Mpa, 45 ℃ of extraction temperature, the entrainer working concentration is 85% alcoholic solution, the addition of alcoholic solution is 35% of oleum lini crude oil or a Semen Lini weight;
It is 80% oleum lini that above-mentioned extract is made linolenic acid purity with the rectifying column fractional distillation;
Get above-mentioned CO
27.5 kilograms of the oleum linis of extraction add 67 gram monoglyceride emulsifyings, 70 ℃ of emulsifying temperatures, the emulsion of rotary viscosity 40MPaS, standby;
Above-mentioned core and wall material are mixed, and through homogenizer (or colloid mill) homogenizing, spray-drying process, dry wind advance machine 170-200 ℃, out-of-machine temperature 60-80 ℃, get alpha-linolenic acid microcapsule after the cooling.
Claims (2)
1, a kind of alpha-linolenic acid microcapsule comprises linolenic acid core and wall material, it is characterized in that the wall material is made up of arabic gum, maltodextrin and modified starch, and its weight ratio is: arabic gum 1, maltodextrin 1-1.5, modified starch 3-10; Core and wall material are 15-30 by weight: 100.
2, a kind of method of making the described alpha-linolenic acid microcapsule of claim 1 is characterized in that comprising the steps:
A prepares the wall material:
(1) will dissolve in water than arabic gum 1 unit of weight, water temperature 60-70 ℃, after the dissolving, again with maltodextrin 1-1.5 unit of weight, fully stirring and evenly mixing is made viscosity 30-40Mpa.s water-soluble macromolecule pastel;
(2) modified starch 3-10 unit of weight is added above-mentioned pastel, mix, homogenizing, standby;
B prepares the alpha-linolenic acid core:
(1) with oleum lini crude oil or Semen Lini supercritical CO
2The extraction alpha-linolenic acid, extracting pressure 30～60Mpa, 40～50 ℃ of extraction temperature, the entrainer working concentration is 75～95% alcoholic solution, the addition of alcoholic solution is 5～60% of oleum lini crude oil or a Semen Lini weight;
(2) above-mentioned extract being made linolenic acid purity with the rectifying column fractional distillation is 60～90% oleum lini;
(3) oleum lini that above-mentioned fractional distillation is made adds monoglyceride emulsifying, and it is standby to make core, and the addition of monoglyceride is 0.5～1.2% of an oleum lini weight, 60～70 ℃ of emulsifying temperatures, emulsion rotary viscosity 35-40MPaS;
C with the core of preparation and wall material by weight 15-30: 100 preparations mix, and stir, and spray-drying process, dry wind advance machine 170-200 ℃, out-of-machine temperature 60-80 ℃, after the cooling linolenic acid microcapsule.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01112968 CN1222278C (en) | 2001-05-23 | 2001-05-23 | Alpha-linolenic acid microcapsule and its preparing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01112968 CN1222278C (en) | 2001-05-23 | 2001-05-23 | Alpha-linolenic acid microcapsule and its preparing process |
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| CN1386497A CN1386497A (en) | 2002-12-25 |
| CN1222278C true CN1222278C (en) | 2005-10-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 01112968 Expired - Fee Related CN1222278C (en) | 2001-05-23 | 2001-05-23 | Alpha-linolenic acid microcapsule and its preparing process |
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Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100348568C (en) * | 2005-10-18 | 2007-11-14 | 中国人民解放军第四军医大学药物研究所 | Process for extracting high purity alpha-linolenic acid from pepper category and medicine application thereof |
| CL2008002157A1 (en) * | 2008-07-23 | 2009-02-20 | Gillot Sandra | Microencapsulated food product rich in omega-3 containing chia oil, dipotassium phosphate, ascorbyl palmitate, alpha-tocopherol, modified starch, maltodextrin, gum arabic; manufacturing process that comprises dispersion of ingredients, homogenization, microencapsulation; applications. |
| CN102071102A (en) * | 2011-01-25 | 2011-05-25 | 唐忠海 | Method for extracting hovenia dulcis thunb.seed oil by using supercritical CO2 technology |
| CN102429215B (en) * | 2011-10-24 | 2013-05-01 | 陈元涛 | Linolenic acid microcapsules and preparation method thereof |
| CN102488079B (en) * | 2011-12-13 | 2013-01-23 | 张绍林 | Composite seal oil microcapsule feed additive and preparation method thereof |
| GB2500673A (en) * | 2012-03-29 | 2013-10-02 | Imran Mohammed | Encapsulated chia oil |
| CN102726548B (en) * | 2012-06-18 | 2013-12-11 | 南京农业大学 | Blackberry seed oil microcapsule and preparation method thereof |
| CN102934703B (en) * | 2012-11-13 | 2015-07-15 | 中国食品发酵工业研究院 | Flaxseed oil microcapsule and production method thereof |
| CN103053910B (en) * | 2013-01-29 | 2014-05-14 | 李太和 | Method for producing omega-3 fatty acid food additive |
| CN103071435B (en) * | 2013-02-01 | 2014-11-05 | 深圳市兰亭科技股份有限公司 | Preparation method of gamma-linolenic acid nano microcapsule |
| CN104522318B (en) * | 2014-12-22 | 2017-12-05 | 新奥（厦门）农牧发展有限公司 | A kind of micro-capsule fat powder for improving the enrichment meat, eggs and milks of Ω 3 and preparation method thereof |
| CN104522666A (en) * | 2015-01-04 | 2015-04-22 | 吉林省农业科学院 | Dahurian rose fruit seed oil and purple perilla seed oil composite microcapsule capable of assisting in reducing blood fat and preparation method thereof |
| CN107019691A (en) * | 2016-02-02 | 2017-08-08 | 广州中医药大学第二附属医院 | Alpha-linolenic acid as 1 type plasminogen activator inhibitor conditioning agent application |
| CN105733802A (en) * | 2016-04-13 | 2016-07-06 | 上海本真食品有限公司 | Flax seed oil capable of reducing high blood pressure, high blood lipid and high blood sugar and preparation method thereof |
| CN105995903A (en) * | 2016-05-11 | 2016-10-12 | 上海旭梅香精有限公司 | Method for preparing chrysanthemum flower spice powder |
| CN108741081A (en) * | 2018-06-29 | 2018-11-06 | 许昌元化生物科技有限公司 | One kind containing linolenic composite micro-powder and preparation method thereof |
| CN108968070A (en) * | 2018-08-13 | 2018-12-11 | 河南城建学院 | A kind of linseed omega-3 unsaturated fatty acid health care product and its microcapsule preparation method |
| CN112167598A (en) * | 2020-10-15 | 2021-01-05 | 吉源(淮北)食品科技有限公司 | Preparation method of microcapsule particle slow-release coating essence |
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2001
- 2001-05-23 CN CN 01112968 patent/CN1222278C/en not_active Expired - Fee Related
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Address after: 201801 room 1, building 2889, No. 103, Baoan Road, Shanghai, Jiading District Patentee after: Shanghai prospect Health Management Co., Ltd. Address before: Jiading District Malu Town, Shanghai City No. 2968 Baoan road 201801 Patentee before: Shanghai prospect Jinxiu Trade Co., Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20051012 Termination date: 20200523 |
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| CF01 | Termination of patent right due to non-payment of annual fee |