CN115005446A - Organic DHA microcapsule powder and preparation method thereof - Google Patents
Organic DHA microcapsule powder and preparation method thereof Download PDFInfo
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- CN115005446A CN115005446A CN202210755845.6A CN202210755845A CN115005446A CN 115005446 A CN115005446 A CN 115005446A CN 202210755845 A CN202210755845 A CN 202210755845A CN 115005446 A CN115005446 A CN 115005446A
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- 239000000843 powder Substances 0.000 title claims abstract description 67
- 239000003094 microcapsule Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 24
- 238000010008 shearing Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 16
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 16
- 238000000265 homogenisation Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 11
- 238000001694 spray drying Methods 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 8
- 239000004519 grease Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 48
- 235000019198 oils Nutrition 0.000 claims description 27
- 235000006708 antioxidants Nutrition 0.000 claims description 12
- 239000001506 calcium phosphate Substances 0.000 claims description 12
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical group [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 9
- 229910000391 tricalcium phosphate Inorganic materials 0.000 claims description 9
- 229940078499 tricalcium phosphate Drugs 0.000 claims description 9
- 235000019731 tricalcium phosphate Nutrition 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 7
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- 229930003427 Vitamin E Natural products 0.000 claims description 5
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 150000003904 phospholipids Chemical class 0.000 claims description 5
- 235000019165 vitamin E Nutrition 0.000 claims description 5
- 229940046009 vitamin E Drugs 0.000 claims description 5
- 239000011709 vitamin E Substances 0.000 claims description 5
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- 239000005862 Whey Substances 0.000 claims description 4
- 102000007544 Whey Proteins Human genes 0.000 claims description 4
- 108010046377 Whey Proteins Proteins 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000001509 sodium citrate Substances 0.000 claims description 4
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 4
- 235000019739 Dicalciumphosphate Nutrition 0.000 claims description 3
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 3
- NEFBYIFKOOEVPA-UHFFFAOYSA-K dicalcium phosphate Chemical compound [Ca+2].[Ca+2].[O-]P([O-])([O-])=O NEFBYIFKOOEVPA-UHFFFAOYSA-K 0.000 claims description 3
- 229910000390 dicalcium phosphate Inorganic materials 0.000 claims description 3
- 229940038472 dicalcium phosphate Drugs 0.000 claims description 3
- 235000021323 fish oil Nutrition 0.000 claims description 3
- 239000008101 lactose Substances 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- 239000006188 syrup Substances 0.000 claims description 3
- 235000020357 syrup Nutrition 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 2
- 235000010323 ascorbic acid Nutrition 0.000 claims description 2
- 239000011668 ascorbic acid Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 241000195493 Cryptophyta Species 0.000 claims 2
- 239000003995 emulsifying agent Substances 0.000 abstract description 5
- 239000003381 stabilizer Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 1
- MBMBGCFOFBJSGT-KUBAVDMBSA-N all-cis-docosa-4,7,10,13,16,19-hexaenoic acid Chemical compound CC\C=C/C\C=C/C\C=C/C\C=C/C\C=C/C\C=C/CCC(O)=O MBMBGCFOFBJSGT-KUBAVDMBSA-N 0.000 description 88
- 235000020669 docosahexaenoic acid Nutrition 0.000 description 47
- 229940090949 docosahexaenoic acid Drugs 0.000 description 44
- 230000001276 controlling effect Effects 0.000 description 17
- 238000004090 dissolution Methods 0.000 description 6
- 150000002978 peroxides Chemical class 0.000 description 6
- 238000012545 processing Methods 0.000 description 5
- DVSZKTAMJJTWFG-SKCDLICFSA-N (2e,4e,6e,8e,10e,12e)-docosa-2,4,6,8,10,12-hexaenoic acid Chemical compound CCCCCCCCC\C=C\C=C\C=C\C=C\C=C\C=C\C(O)=O DVSZKTAMJJTWFG-SKCDLICFSA-N 0.000 description 3
- GZJLLYHBALOKEX-UHFFFAOYSA-N 6-Ketone, O18-Me-Ussuriedine Natural products CC=CCC=CCC=CCC=CCC=CCC=CCCCC(O)=O GZJLLYHBALOKEX-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- KAUVQQXNCKESLC-UHFFFAOYSA-N docosahexaenoic acid (DHA) Natural products COC(=O)C(C)NOCC1=CC=CC=C1 KAUVQQXNCKESLC-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000008213 purified water Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 229930003231 vitamin Natural products 0.000 description 3
- 239000011782 vitamin Substances 0.000 description 3
- 229940088594 vitamin Drugs 0.000 description 3
- 235000013343 vitamin Nutrition 0.000 description 3
- 150000003722 vitamin derivatives Chemical class 0.000 description 3
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 235000013373 food additive Nutrition 0.000 description 2
- 239000002778 food additive Substances 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 235000013348 organic food Nutrition 0.000 description 2
- 241001494479 Pecora Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000601 blood cell Anatomy 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 230000004641 brain development Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 235000013350 formula milk Nutrition 0.000 description 1
- 239000009153 huxin Substances 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000020660 omega-3 fatty acid Nutrition 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 210000001525 retina Anatomy 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
- A23L33/12—Fatty acids or derivatives thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/20—Agglomerating; Granulating; Tabletting
- A23P10/28—Tabletting; Making food bars by compression of a dry powdered mixture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Mycology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses organic DHA microcapsule powder and a preparation method thereof. The DHA powder comprises the following components in percentage by mass: 25.0 to 30.0 percent of DHA, 65 to 72 percent of dispersant, 0.1 to 0.3 percent of acidity regulator, 0.1 to 0.3 percent of water-soluble antioxidant, 1.5 to 3.4 percent of oil-soluble antioxidant and 0.5 to 1 percent of anticaking agent. The preparation method comprises the following steps: dissolving a dispersing agent, an acidity regulator and a water-soluble antioxidant in water to serve as a dispersion phase, mixing DHA grease and the oil-soluble antioxidant to serve as an oil phase, mixing the dispersion phase and the oil phase, grinding, sequentially performing high-speed shearing, high-pressure homogenization and spray drying, and mixing with an anticaking agent after drying. According to the invention, on the premise of not adding a chemical emulsifier and a stabilizer, the effective embedding technology of the nano microcapsule is realized through high-speed grinding, high-speed shearing and high-pressure homogenizing processes, and the prepared organic DHA powder product has the advantages of low surface oil and good stability.
Description
Technical Field
The invention belongs to the technical field of microencapsulated nutritional products, and particularly relates to organic docosahexaenoic acid (DHA) microcapsule powder and a preparation method thereof.
Background
Docosahexaenoic acid (DHA) belongs to omega-3 series fatty acid, is an important constituent component of infant brain development and retina, has a series of physiological functions of softening blood vessels, reducing cholesterol, regulating blood cells and the like for old people, and has increasingly significant nutritional value and commercial significance.
At present, in order to ensure a good emulsifying effect, a plurality of DHA products need to be added with chemically synthesized emulsifiers and the like in the processing process, so that the products cannot be sold as 'organic food'. For example, chinese patent CN107660620B discloses a sheep oil-based lipid microcapsule powder, CN103549442B a DHA algal oil microcapsule powder with high oil loading, which uses non-organic materials as wall materials and chemically synthesized food additives (emulsifiers), and thus does not meet the requirements of organic certification regulations. With the rapid development of organic agriculture and organic product processing industry all over the world, the demand of organic DHA powder products is increasing, and therefore, the development of organic DHA powder products has great potential.
Due to the regulation and restriction of organic product processing, a lot of non-organic raw and auxiliary materials and food additives with good emulsifying and embedding effects cannot be added and used at will, so that the real organic DHA product has poor stability and extremely short shelf life, and is not beneficial to long-distance transportation and terminal sale.
Disclosure of Invention
In view of the deficiencies of the prior art and the associated requirements and limitations of the regulations, it is an object of the present invention to provide a docosahexaenoic acid (DHA) powder and a process for its preparation that is simple in handling steps and fully meets the requirements of the regulations for organic agricultural processes in europe, the usa, japan, etc.
In order to achieve the technical purpose, the inventor of the present invention has diligently tried and studied through a large amount of experiments, and finally, the nano microcapsule embedding of DHA is achieved by replacing the action of chemical emulsifier and stabilizer through high-speed grinding, high-speed shearing and high-pressure homogenizing processes, and the following technical solutions are obtained: the organic DHA microcapsule powder comprises the following components in percentage by mass:
the dispersing agent is selected from one or a mixture of more than two of organic whey powder, organic lactose, organic glucose syrup, organic glucose and organic starch;
the acidity regulator is one or two of citric acid, sodium citrate and sodium hydroxide;
the water-soluble antioxidant is selected from ascorbic acid which meets organic regulation;
the oil-soluble antioxidant is selected from one or two of organic phospholipid and vitamin E (meeting organic regulation);
the preparation method of the organic DHA microcapsule powder comprises the following steps: dissolving a dispersing agent, an acidity regulator and a water-soluble antioxidant in water at 60-70 ℃ to serve as a dispersion phase, mixing DHA grease and the oil-soluble antioxidant, keeping the temperature at 60-70 ℃ to serve as an oil phase, mixing the dispersion phase and the oil phase, grinding the mixture at 25-35 ℃ until the particle size is less than 300nm, sequentially carrying out high-speed shearing, high-pressure homogenization and spray drying, and mixing with the anticaking agent to obtain organic DHA microcapsule powder.
Further preferably, the organic DHA microcapsule powder as described above, wherein the DHA oil may be oil of microalgae fermentation source, such as DHA algal oil, more specifically, organic DHA algal oil of fermentation source, for example, manufactured by north huxin and biotechnology limited; it may also be a naturally occurring organic oil such as DHA fish oil.
Further preferably, the organic DHA microcapsule powder as described above, wherein the anti-caking agent is selected from tricalcium phosphate, dicalcium phosphate, which complies with the organic regulations.
Further preferably, the organic DHA microcapsule powder is prepared by the method described above, wherein the shearing speed of the high-speed shearing step is 30000 r/min-40000 r/min, and the shearing time is 25-35 min.
Further preferably, the organic DHA microcapsule powder as described above, wherein the pressure of the high pressure homogenization step is: homogenizing for 2-3 times, wherein the primary pressure is 6-10 MPa, the secondary pressure is 60-80 MPa.
In addition, the invention also provides a preparation method of the organic DHA microcapsule powder, which comprises the following steps:
(1) preparation of dispersed phase: weighing a dispersing agent, an acidity regulator and a water-soluble antioxidant, dissolving in water at 60-70 ℃, fully dissolving, and then preserving heat for 25-35 min;
(2) preparing an oil phase: weighing DHA grease and an oil-soluble antioxidant, uniformly mixing, heating to 60-70 ℃, and keeping the temperature for 25-35 min;
(3) mixing the oil phase prepared in the step (2) with the dispersed phase prepared in the step (1), and cooling the mixed material to 25-35 ℃ for later use;
(4) conveying the material obtained in the step (3) to a high-speed grinding machine for grinding for 1-2 h, wherein the grinding speed is 5000-10000 r/min, the temperature of the material is controlled at 25-35 ℃, and grinding is stopped when the particle size is smaller than 300 nm;
(5) shearing the ground material in the step (4) at a high speed of 30000 r/min-40000 r/min for 25-35 min;
(6) and (3) carrying out high-pressure homogenization on the sheared material in the step (5), controlling the temperature of the material to be 50-60 ℃, and controlling the pressure of the high-pressure homogenization to be as follows: homogenizing for 2-3 times under the primary pressure of 6-10 MPa and the secondary pressure of 60-80 MPa, and then carrying out spray drying;
(7) and (4) mixing the powder obtained in the step (6) with an anticaking agent at the rear end of the fluidized bed to obtain organic DHA microcapsule powder with good fluidity.
Further preferably, in the preparation method of the organic DHA microcapsule powder, the air inlet temperature adopted in the spray drying in the step (6) is 150-160 ℃, and the air outlet temperature is 65-75 ℃.
Compared with the prior art, the DHA microcapsule powder and the preparation method thereof provided by the invention have the following advantages and remarkable progresses:
(1) the raw materials used in the invention are all organic raw materials or non-organic raw materials allowed by organic production and processing laws, so that the DHA product meets the organic certification standard and fills the gap of domestic organic DHA products.
(2) According to the invention, on the premise of not adding a chemical emulsifier and a stabilizer, the effective embedding technology of the nano microcapsule is realized through high-speed grinding, high-speed shearing and high-pressure homogenizing processes, and the prepared organic DHA powder product has the advantages of low surface oil and good stability.
(3) The invention has simple process flow and is suitable for industrial scale production, and the prepared DHA powder meets the production and processing requirements of organic products such as Europe, America, Japan and the like, so that the DHA powder can be used for preparing organic infant formula milk powder and other organic foods meeting relevant regulations.
Detailed Description
The present invention is further illustrated by the following detailed description, wherein the technical steps or conditions not specified in the examples are performed according to the technical or conditions described in the literature in the field or according to the product specification. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
Preparing organic DHA microcapsule powder according to the following steps:
dissolving 125kg of weighed organic whey powder, 1.2kg of sodium citrate, 261.5kg of organic glucose syrup and vitamin C1kg in 780kg of purified water at 60-70 ℃, and preserving heat for 30min after full dissolution to obtain a material A for later use;
weighing 150kg of organic DHA grease, 11.4kg of organic phospholipid and 1.5kg of vitamin E, heating, dissolving and mixing, controlling the temperature to be 60-70 ℃ after full dissolution, and keeping the temperature for 30min to obtain a material B for later use;
fully mixing the material A and the material B, and reducing the temperature of the materials to 25-35 ℃; then grinding for 1-2 h in a started high-speed grinding machine, controlling the rotation number of the grinding machine at a grinding speed of 5000r/min, controlling the temperature of the material at 25-35 ℃, stopping grinding when the particle size of the material is smaller than 300nm through detection of a laser particle size tester, and properly prolonging the grinding time if necessary to obtain a material C for later use;
shearing the material C at a high speed of 30000 r/min-40000 r/min for 30min, and after shearing, carrying out high-pressure homogenization for 2 times, wherein the primary pressure is controlled to be 8MPa, and the secondary pressure is controlled to be 60 MPa; controlling the temperature of the material at 50-60 ℃ to obtain a material D for later use;
and (3) spray-drying the material D, controlling the air inlet temperature to be 150-160 ℃ and the air outlet temperature to be 65-75 ℃ to obtain organic DHA powder, and adding 2.8kg of tricalcium phosphate when the powder passes through the rear end of the fluidized bed and fully mixing with the tricalcium phosphate to obtain the organic DHA powder with good fluidity.
The powder has surface oil of 0.05% and powder peroxide value of 0 mmol/kg; the result of the high-temperature stability test at 62 ℃ shows that the surface oil of the powder is 0.05 percent after 58 days, and the peroxide value is 0.25mmol/kg, which indicates that the stability of the organic DHA powder produced by the process is better than that of a non-organic product. The shelf life of the product produced by the method is more than 24 months.
Example 2
Preparing organic microcapsule DHA powder according to the following steps:
dissolving 100kg of weighed organic whey powder, 1.2kg of sodium citrate, 286.5kg of organic lactose and 1kg kg of vitamin C1 in 780kg of purified water at 60-70 ℃, and preserving heat for 30min after full dissolution to obtain a material A for later use;
weighing 150kg of organic DHA grease, 11.4kg of organic phospholipid and 1.5kg of vitamin E, heating, dissolving and mixing, controlling the temperature to be 60-70 ℃ after full dissolution, and keeping the temperature for 30min to obtain a material B for later use;
fully mixing the material A and the material B, and reducing the temperature of the materials to 25-35 ℃; then grinding for 1-2 h in a started high-speed grinding machine, controlling the rotation number of the grinding machine at 8000r/min, controlling the temperature of the material at 25-35 ℃, and stopping grinding when the particle size is smaller than 300nm through detection of a laser particle size tester to obtain a material C for later use;
shearing the material C at a high speed of 30000 r/min-40000 r/min for 30min, and after shearing is finished, carrying out high-pressure homogenization for 2 times, wherein the primary pressure is controlled to be 8MPa, and the secondary pressure is controlled to be 70 MPa; controlling the temperature of the material at 50-60 ℃ to obtain a material D for later use;
and (3) spray-drying the material D, controlling the air inlet temperature to be 150-160 ℃ and the air outlet temperature to be 65-75 ℃ to obtain organic DHA powder, and adding 2.8kg of tricalcium phosphate when the powder passes through the rear end of the fluidized bed and fully mixing with the tricalcium phosphate to obtain the organic DHA powder with good fluidity.
The powder has surface oil of 0.02% and powder peroxide value of 0 mmol/kg; the result of a high-temperature stability test at 62 ℃ shows that the surface oil of the powder is 0.02 percent after 58 days, and the peroxide value is 0.21mmol/kg, which indicates that the stability of the organic DHA powder produced by the process is better than that of a non-organic product. The shelf life of the product produced by the method is more than 24 months.
Example 3
Preparing organic microcapsule DHA powder according to the following steps:
dissolving 120kg of weighed organic starch, 1.2kg of citric acid, 291.5kg of organic glucose and 1kg of vitamin C1 in 780kg of purified water at 60-70 ℃, and preserving heat for 30min after full dissolution to obtain a material A for later use;
weighing 150kg of organic DHA grease, 11.4kg of organic phospholipid and 1.5kg of vitamin E, heating, dissolving and mixing, controlling the temperature to be 60-70 ℃ after full dissolution, and keeping the temperature for 30min to obtain a material B for later use;
fully mixing the material A and the material B, and reducing the temperature of the materials to 25-35 ℃; then grinding for 1-2 h in a started high-speed grinding machine, controlling the rotation number of the grinding machine at 8000r/min, controlling the temperature of the material at 25-35 ℃, and stopping grinding when the particle size is smaller than 300nm through detection of a laser particle size tester to obtain a material C for later use;
shearing the material C at a high speed of 30000 r/min-40000 r/min for 30min, and after shearing, carrying out high-pressure homogenization for 2 times, wherein the primary pressure is controlled to be 8MPa, and the secondary pressure is controlled to be 80 MPa; controlling the temperature of the material at 50-60 ℃ to obtain a material D for later use;
and (3) spray-drying the material D, controlling the air inlet temperature to be 150-160 ℃ and the air outlet temperature to be 65-75 ℃ to obtain organic DHA powder, and adding 2.8kg of tricalcium phosphate when the powder passes through the rear end of the fluidized bed and fully mixing with the tricalcium phosphate to obtain the organic DHA powder with good fluidity.
The powder has surface oil of 0.03% and powder peroxide value of 0 mmol/kg; the result of a high-temperature stability test at 62 ℃ shows that the surface oil of the powder is 0.03 percent after 58 days, and the peroxide value is 0.21mmol/kg, which indicates that the stability of the organic DHA powder produced by the process is better than that of a non-organic product. The shelf life of the product produced by the method is more than 24 months.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof should be equivalent or changed within the scope of the present invention.
Claims (9)
1. The organic DHA microcapsule powder is characterized by comprising the following components in percentage by mass:
the dispersing agent is selected from one or a mixture of more than two of organic whey powder, organic lactose, organic glucose syrup, organic glucose and organic starch;
the acidity regulator is selected from one or two of citric acid, sodium citrate and sodium hydroxide;
the water-soluble antioxidant is selected from ascorbic acid;
the oil-soluble antioxidant is selected from one or two of organic phospholipid and vitamin E;
the preparation method comprises the following steps: dissolving a dispersing agent, an acidity regulator and a water-soluble antioxidant in water at 60-70 ℃ to serve as a dispersion phase, mixing DHA grease and the oil-soluble antioxidant, keeping the temperature at 60-70 ℃ to serve as an oil phase, mixing the dispersion phase and the oil phase, grinding the mixture at 25-35 ℃ until the particle size is less than 300nm, sequentially carrying out high-speed shearing, high-pressure homogenization and spray drying, and mixing with the anticaking agent to obtain organic DHA microcapsule powder.
2. An organic DHA microcapsule powder according to claim 1, wherein the DHA oil is selected from one or more of the following: DHA algae oil and DHA fish oil.
3. An organic DHA microcapsule powder according to claim 1, wherein the anti-caking agent is selected from tricalcium phosphate, dicalcium phosphate, which complies with the organic regulations.
4. The organic DHA microcapsule powder according to claim 1, wherein the shearing speed in the high-speed shearing step is 30000r/min to 40000r/min, and the shearing time is 25 to 35 min.
5. An organic DHA microcapsule powder according to claim 1, wherein the pressure of the high pressure homogenization step is: homogenizing for 2-3 times under the primary pressure of 6-10 MPa and the secondary pressure of 60-80 MPa.
6. A process for the preparation of an organic DHA microcapsule powder according to claim 1, comprising the steps of:
(1) preparation of dispersed phase: weighing a dispersing agent, an acidity regulator and a water-soluble antioxidant, dissolving in water at 60-70 ℃, fully dissolving, and then preserving heat for 25-35 min;
(2) preparing an oil phase: weighing DHA grease and an oil-soluble antioxidant, uniformly mixing, heating to 60-70 ℃, and keeping the temperature for 25-35 min;
(3) mixing the oil phase prepared in the step (2) with the dispersed phase prepared in the step (1), and cooling the mixed material to 25-35 ℃ for later use;
(4) conveying the material obtained in the step (3) to a high-speed grinding machine for grinding for 1-2 h, wherein the grinding speed is 5000-10000 r/min, the temperature of the material is controlled at 25-35 ℃, and grinding is stopped when the particle size is smaller than 300 nm;
(5) shearing the ground material in the step (4) at a high speed of 30000 r/min-40000 r/min for 25-35 min;
(6) and (3) carrying out high-pressure homogenization on the sheared material in the step (5), controlling the temperature of the material to be 50-60 ℃, and controlling the pressure of the high-pressure homogenization to be as follows: homogenizing for 2-3 times under the primary pressure of 6-10 MPa and the secondary pressure of 60-80 MPa, and then carrying out spray drying;
(7) and (4) mixing the powder obtained in the step (6) with an anticaking agent at the rear end of the fluidized bed to obtain organic DHA microcapsule powder with good fluidity.
7. The preparation method of organic DHA microcapsule powder according to claim 6, wherein the air inlet temperature adopted in the spray drying in the step (6) is 150-160 ℃ and the air outlet temperature is 65-75 ℃.
8. The method for preparing organic DHA microcapsule powder according to claim 6, wherein the DHA oil is selected from one or more of the following: DHA algae oil and DHA fish oil.
9. The method for preparing organic DHA microcapsule powder according to claim 6, wherein the anticaking agent is selected from tricalcium phosphate and dicalcium phosphate which meet organic regulations.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105707894A (en) * | 2016-04-01 | 2016-06-29 | 广东润科生物工程有限公司 | Preparation method of high-temperature-resistant microalgae DHA (docosahexenoic acid) oil microcapsule powder |
| CN111685190A (en) * | 2020-06-06 | 2020-09-22 | 青岛海智源生命科技有限公司 | Nano-scale DHA algae oil powder and emulsification preparation method thereof |
| CN114041601A (en) * | 2021-12-06 | 2022-02-15 | 润科生物工程（福建）有限公司 | Process for preparing DHA microcapsule powder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105707894A (en) * | 2016-04-01 | 2016-06-29 | 广东润科生物工程有限公司 | Preparation method of high-temperature-resistant microalgae DHA (docosahexenoic acid) oil microcapsule powder |
| CN111685190A (en) * | 2020-06-06 | 2020-09-22 | 青岛海智源生命科技有限公司 | Nano-scale DHA algae oil powder and emulsification preparation method thereof |
| CN114041601A (en) * | 2021-12-06 | 2022-02-15 | 润科生物工程（福建）有限公司 | Process for preparing DHA microcapsule powder |
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