CN117137143A - Stable sheep-based unsaturated fatty acid grease microcapsule powder and preparation method thereof - Google Patents
Stable sheep-based unsaturated fatty acid grease microcapsule powder and preparation method thereof Download PDFInfo
- Publication number
- CN117137143A CN117137143A CN202311180083.2A CN202311180083A CN117137143A CN 117137143 A CN117137143 A CN 117137143A CN 202311180083 A CN202311180083 A CN 202311180083A CN 117137143 A CN117137143 A CN 117137143A
- Authority
- CN
- China
- Prior art keywords
- fatty acid
- sheep
- unsaturated fatty
- microcapsule powder
- based unsaturated
- Prior art date
- 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.)
- Pending
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- 239000004519 grease Substances 0.000 title claims abstract description 49
- 239000003094 microcapsule Substances 0.000 title claims abstract description 47
- 241001494479 Pecora Species 0.000 title claims abstract description 44
- 235000021122 unsaturated fatty acids Nutrition 0.000 title claims abstract description 35
- 150000004670 unsaturated fatty acids Chemical class 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
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- 125000005456 glyceride group Chemical group 0.000 claims description 34
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid group Chemical group C(CC(O)(C(=O)O)CC(=O)O)(=O)O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 30
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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
-
- 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
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
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- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
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Abstract
The invention belongs to the field of manufacturing of compound food additives. The invention discloses stable sheep-based unsaturated fatty acid grease microcapsule powder and a preparation method thereof, wherein the microcapsule powder comprises the following components in percentage by mass: 40.91 to 92.5 percent of wall material; 5% -50% of core material treated by a special process; 2.5 to 8 percent of antioxidant; 0 to 0.99 percent of emulsifying agent; 0 to 0.1 percent of acidity regulator; the wall material includes protein and carbohydrate. The protein is entirely derived from the goat milk, the carbohydrate is derived from the goat milk or derived from plants, the stability of the core material is greatly enhanced through special process treatment, the wall material of the cow milk source is avoided, the stability of the goat-based unsaturated fatty acid grease microcapsule powder is greatly improved, the quality requirement of the infant goat milk formula milk powder manufacturer is met, and the technical blank is filled.
Description
Technical Field
The invention relates to the field of infant formula food, and provides stable sheep-based unsaturated fatty acid grease microcapsule powder and a preparation method thereof.
Background
Arachidonic acid (ARA) is one of the important polyunsaturated fatty acids constituting phospholipids in the cerebral cortex, plays an important role in brain development of infants, is an important and direct precursor substance for synthesizing human prostaglandins and various eicosane derivatives with special physiological activities, is called as three-major fatty acids necessary for the human body together with linoleic acid and linolenic acid, and has excellent nutritive value (arachidonic acid application and research progress, once Yu). The lack of ARA has limited cognitive ability and mental development in infants and has low ARA synthesis ability, so that it is necessary to add ARA to infant food to ensure healthy development of infants.
Docosahexaenoic acid (DHA) is a polyunsaturated fatty acid of omega-3 system essential for human body, and has effects of relieving brain diseases, resisting inflammation and cancer, enhancing immunity, enhancing lipid metabolism, and maintaining intestinal tract and cardiovascular health. DHA can promote brain and eye nerve development, and strengthen early cognitive and motor development of infants, and is often used as infant formula milk powder and food additive. DHA from microalgae is widely utilized due to the advantages of simple structure, easy absorption and the like (the influence factor of the stability of docosahexaenoic acid microalgae oil emulsion, du Jian).
Breast milk fat provides more than 50% of energy for infants during their development, and plays a key role in the absorption of multiple vitamins and minerals, which is a nutritional indicator of particular concern in infant formula design. The infant formula is mainly prepared according to the proportion of breast milk fatty acid, so that polyunsaturated fatty acid (such as linoleic acid and alpha-linolenic acid) is properly supplemented to meet the needs of infants. The sunflower seed oil is high-quality edible vegetable oil prepared by oil extraction processes such as squeezing sunflower seeds, is rich in nutrition, contains linoleic acid and oleic acid, the content of which can reach 62.2% and 23.8% respectively, further contains sterols and various minerals, and is rich in tocopherol (about 74.3mg/100 g), wherein alpha-tocopherol accounts for 96.7% of the total tocopherol content, and about 71.84mg/100g (research progress of volatile flavor substances of the sunflower seed oil, yin Wenting). The sunflower seed oil has the health care effects of resisting oxidation, resisting cancer and preventing various diseases.
DHA grease and ARA grease are long-chain polyunsaturated fatty acids, are extremely easy to oxidize, generate hydroperoxides after oxidation, then break and decompose, generate a series of volatile and non-volatile substances with short carbon chains, such as aldehydes, ketones, alcohols, acid substances and the like, lead the grease to have fishy smell, and possibly cause damage to human health, thereby influencing the application of the DHA grease and the ARA grease.
The microcapsule technology is a technology which uses a polymer material as a wall material to wrap a core component to protect a core material, can prolong and control the release of active substances in the microcapsule, and is widely applied to the fields of biology, food, pharmacy, cosmetics and the like. The microcapsule technology is a core means for slowing down the oxidation of grease at present, liquid grease forms solid powder with uniform particles after microencapsulation treatment, the grease sealed in a wall material is isolated from oxidation promoting factors in the environment, the oxidation problem can be effectively avoided, the stability of the product is improved, the shelf life of the product is prolonged, the grease can be added and applied to food with stable quality, meanwhile, the appearance form of the product is changed, so that the product is convenient to carry and transport, and the application range of the product is widened (the preparation of the schizochytrium oil microcapsule powder and the research on oxidation stability, lin Rongfang). Secondly, the microcapsule technology can mask the peculiar smell of the grease to a certain extent, so that the product is more acceptable to the market.
The goat milk is widely accepted dairy products closest to human breast milk in the world, does not contain allergic abnormal casein, is rich in adenosine triphosphate, can promote the decomposition and conversion utilization of lactose in human intestinal tracts, is not easy to produce lactose intolerance phenomenon after drinking, has higher nutritive value compared with cow milk, is more beneficial to human absorption, and is suitable for various special people to eat. At present, infant milk powder in the market is still used as a base, but the quality and the nutritional value of cow milk are reduced because a large amount of antibiotics are used for inhibiting cow mastitis in the cow breeding process, and researches have shown that in infants with the same delivery mode and the same month age, the intestinal flora of infants fed with the infant milk powder is more various, and the abundance of main dominant bacteria is higher (the infant milk powder has an influence on the intestinal flora of the infants and main beneficial bacteria, yang Li). From the aspects of nutrition, health value and the like, the goat milk is a major substrate for infant milk powder in the future. Therefore, it is necessary to develop grease microcapsule powder with goat milk component as main wall material to match with the market development of goat-based milk powder.
Sheep-based unsaturated fatty acid grease microcapsules exist on the market, but the problems of general actual embedding effect and general stability exist.
Disclosure of Invention
The invention aims to solve the technical problem of providing stable sheep-based unsaturated fatty acid grease microcapsule powder and a preparation method thereof, which can improve the situation that the formula stability of the existing DHA and ARA sheep-based powder in the market is slightly insufficient.
The technical aim of the invention is realized by the following technical scheme: the stabilized sheep-based unsaturated fatty acid grease microcapsule powder comprises the following components in percentage by mass:
40.91 to 92.5 percent of wall material;
5% -50% of core material;
2.5 to 8 percent of antioxidant;
0 to 0.99 percent of emulsifying agent;
0 to 0.1 percent of acidity regulator;
the wall material comprises sheep-derived proteins and plant-derived carbohydrates;
the core material comprises polyunsaturated fatty acid grease treated by a special process or polyunsaturated fatty acid grease blended by sunflower seed oil treated by a special process;
the antioxidants include aqueous phase antioxidants and oil phase antioxidants;
the emulsifier comprises an aqueous phase emulsifier and an oil phase emulsifier. .
The invention is further provided with: the polyunsaturated fatty acid grease, namely the core material, is prepared by the following steps:
s1, catalyzing ethyl esterification, namely adding alkali and ethanol into polyunsaturated fatty acid glyceride with the content of 25-30%, wherein the mass ratio of the ethanol to the polyunsaturated fatty acid glyceride is 1.0-1.2, and catalyzing the ethyl esterification, wherein the reaction temperature is 65-70 ℃;
s2, molecular distillation is carried out, and the distillation temperature is 100-110 ℃;
s3, transesterification, namely adding lipase into the distilled polyunsaturated fatty acid glyceride, wherein the transesterification temperature is 50-60 ℃;
s4, performing secondary molecular distillation at the temperature of 215-255 ℃ to obtain unsaturated fatty glyceride with the content of 40-50%.
By adopting the technical scheme, the esterification of polyunsaturated fatty acids with the content of 25-30% is converted from triglyceride form (ethyl ester of different fatty acids obtained by reaction with ethanol) to ethyl ester form. The different fatty acids include unsaturated fatty acids and saturated fatty acids.
First molecular distillation purpose: removing a part of saturated fatty acid ethyl ester byproducts and removing oxidation products of unsaturated fatty acids.
Transesterification purpose: the unsaturated fatty acid ethyl ester is converted into unsaturated fatty acid glyceride.
Again for molecular distillation purposes: and removing unsaturated fatty acid oxidation products again and removing partial saturated fatty acid glyceride to obtain unsaturated fatty acid glyceride with 40-45% content. The content of polyunsaturated fatty glyceride can be improved from 25-30% to more than 40% through transesterification and secondary molecular distillation, and the polyunsaturated fatty glyceride with the content of more than 50% is not stabilized by the polyunsaturated fatty glyceride with the content of 40-45%. The load of the subsequent deodorization working section can be reduced after polyunsaturated fatty acid oxidation products are removed in advance through secondary molecular distillation.
The invention is further provided with: and (2) carrying out low-temperature short-time deodorization on the unsaturated fatty glyceride with the content of 40-50% obtained in the step (S4), wherein the deodorization condition is that the temperature is 170 ℃, the time is 45-65 min, and the residual pressure is high: and (3) adding a chelating agent and an oil-soluble antioxidant into the deodorized polyunsaturated fatty acid glyceride at 230-235 Pa.
By adopting the technical scheme, the temperature and time for heat treatment of unsaturated fatty glyceride in the deodorization procedure are shortened.
The invention is further provided with: the chelating agent is citric acid.
By adopting the technical scheme, the citric acid can chelate metal ions, so that the oxidation speed is reduced, and the shelf life of grease is prolonged. The unsaturated fatty acid oil and fat has an oxidation rate 100 to 1000 times higher in the presence of a high metal ion concentration than in the absence or presence of a low metal ion concentration.
The invention is further provided with: the sheep-derived protein is one or more of defatted sheep milk powder, sheep concentrated whey protein, sheep isolated whey protein, sheep casein, and sheep desalted whey powder.
The invention is further provided with: the plant-derived carbohydrate is selected from one or two of maltodextrin, maltose, solid corn syrup and goat lactose.
The invention is further provided with: the core material is one or a mixture of more than one of DHA grease, ARA grease and sunflower seed oil.
The invention is further provided with: the water phase antioxidant is sodium ascorbate; the oil phase antioxidant is one or two of ascorbyl palmitate, vitamin E and phospholipid.
The invention is further provided with: the water phase emulsifier is one or two of fatty acid ester of mono-diglycerol and fatty acid glyceride of citric acid; the oil phase emulsifier is phospholipid.
The invention is further provided with: the acidity regulator is one or two of citric acid, sodium citrate, dipotassium hydrogen phosphate, disodium hydrogen phosphate and sodium dihydrogen phosphate.
A method for preparing the stabilized sheep-based unsaturated fatty acid grease microcapsule powder according to claim 1, which is characterized in that: the preparation method comprises the following steps:
(1) Preparing an aqueous phase: weighing wall material, water phase antioxidant, water phase emulsifier and acidity regulator, dissolving in pure water at 50-65 deg.c, stirring to mix completely;
(2) Preparing an oil phase: weighing the core material treated by the special process, thawing in water bath, and adding an oil phase antioxidant, wherein the oil phase antioxidant comprises an oil phase emulsifier, uniformly mixing, and shearing for 1-30 min by using a high-efficiency shearing machine until the temperature of the oil phase is increased by 1-5 ℃;
(3) Pumping the oil phase prepared in the step (2) into the water phase prepared in the step (1), and pre-homogenizing by using a high-speed shearing machine to disperse the oil phase in the water phase to form emulsion;
(4) Homogenizing the emulsion prepared in the step (3) for 1-2 times;
(5) Pasteurizing or high-temperature instantaneous sterilizing the homogenized emulsion in the step (4);
(6) And (3) carrying out spray drying on the feed liquid in the step (5) to obtain the stabilized sheep-based unsaturated fatty acid grease microcapsule powder.
The invention is further provided with: in the step (1), the weight of the pure water is 1 to 1.6 times of the total weight of the microcapsule powder.
The invention is further provided with: in the step (4), the homogenizing pressure is 25-45 MPa, and the second homogenizing pressure can be equal to or slightly lower than the first homogenizing pressure when the material is homogenized.
The invention is further provided with: in the step (5), the pasteurization temperature is 60-70 ℃, the pasteurization time is 30-35 min or 80 ℃ and 15-30S are sterilized instantaneously.
The invention is further provided with: in the step (6), the air inlet temperature adopted by the spray drying is 160-180 ℃ and the air outlet temperature is 70-90 ℃.
The beneficial effects of the invention are as follows:
1. the protein in the invention is all derived from the goat milk, the carbohydrate is derived from plants, no cow milk derived wall material exists, and the requirements of the infant goat milk formula milk powder are completely met.
2. Compared with the existing products on the market, the core material of the invention is treated by a series of special processes, the addition of the antioxidant, especially the addition of sodium ascorbate, is greatly improved, the use level of the emulsifier, especially the aqueous phase emulsifier, is greatly reduced, the oxidation resistance of ARA, especially DHA, in the oil phase is improved by adding sunflower seed oil, the actual embedding effect of the obtained microcapsule is excellent, the shelf life stability of the product is greatly enhanced, the current situations of general actual embedding effect and general stability of the sheep-based microcapsule grease powder are improved, and the market blank of the steady sheep-based unsaturated fatty acid microcapsule product is filled.
3. The wall material is suitable for embedding DHA grease and ARA grease, and is also suitable for embedding one or more unsaturated fatty acid mixed grease.
Detailed Description
The technical solutions in the embodiments will be clearly and completely described below. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
Example 1
In this example, the method for preparing stabilized Yang Ji ARA microcapsule powder comprises the steps of:
(1) Preparing an aqueous phase: 41kg of wall material defatted goat milk powder and 31.8kg of maltodextrin are weighed, 3kg of aqueous antioxidant sodium ascorbate is weighed, 0.1kg of aqueous emulsifier mono-diglycerol fatty acid ester is weighed, 10g of acidity regulator sodium citrate is weighed, dissolved in pure water of 150kg at 65 ℃ and stirred until the mixture is completely dissolved.
(2) Preparing an oil phase: 24kg of core ARA grease treated by a special process, 80g of oil phase antioxidant ascorbyl palmitate, 14.4g of vitamin E and 14.4g of oil phase emulsifier phospholipid are weighed and uniformly mixed.
(3) Adding the oil phase prepared in the step (2) into the water phase prepared in the step (1), and pre-homogenizing by using a shearing machine to obtain an emulsion.
(4) Homogenizing the emulsion prepared in the step (3) for 2 times by using a homogenizer, wherein the homogenizing pressure is 35MPa for the first time and 32MPa for the second time.
(5) And (3) pasteurizing the homogenized material in the step (4) under the pasteurization condition of 68 ℃ for 30min.
(6) Spray drying the pasteurized material at 168 ℃ and 82 ℃ to obtain sheep-based ARA microcapsule powder.
The polyunsaturated fatty acid grease is treated by adopting a special process, and the treatment method comprises the following steps:
s1, catalyzing ethyl esterification, namely adding alkali and ethanol into polyunsaturated fatty acid glyceride with the content of 25-30%, wherein the mass ratio of the ethanol to the polyunsaturated fatty acid glyceride is 1.2, and catalyzing the ethyl esterification, wherein the reaction temperature is 65-70 ℃;
s2, molecular distillation is carried out, and the distillation temperature is 100-110 ℃;
s3, transesterification, namely adding lipase into the distilled polyunsaturated fatty acid glyceride, wherein the transesterification temperature is 50-60 ℃;
s4, performing secondary molecular distillation at the temperature of 215-255 ℃ to obtain unsaturated fatty glyceride with the content of 40-50%.
And (2) carrying out low-temperature short-time deodorization on the unsaturated fatty glyceride with the content of 40-50% obtained in the step (S4), wherein the deodorization condition is that the temperature is 170 ℃, the time is 45-65 min, and the residual pressure is high: 230 to 235Pa, adding nitrogen into the deodorized polyunsaturated fatty acid glyceride, and then adding citric acid and an oil-soluble antioxidant.
The detection shows that the peroxide value of the surface oil is 0.21%, and the anisole value is 0.1 after 46 days of destructive test at 60 ℃ and 1.5 mmol/kg.
Example 2
In this embodiment, the method for preparing stabilized Yang Ji DHA microcapsule powder comprises the following steps:
(1) Preparing an aqueous phase: 40.5kg of wall material defatted goat milk powder and 28.9kg of maltodextrin are weighed, 4.3kg of aqueous antioxidant sodium ascorbate is weighed, 0.1kg of aqueous emulsifier mono-diglycerol fatty acid ester is weighed, 10g of acidity regulator sodium citrate is weighed, dissolved in 150kg of pure water at 65 ℃, and stirred until complete dissolution.
(2) Preparing an oil phase: 24kg of DHA grease of a core material treated by a special process, 2kg of sunflower seed oil, 105.6g of ascorbyl palmitate of an oil phase antioxidant, 19.2g of vitamin E and 36g of phospholipid of an oil phase emulsifier are weighed and uniformly mixed.
(3) Adding the oil phase prepared in the step (2) into the water phase prepared in the step (1), and pre-homogenizing by using a shearing machine to obtain an emulsion.
(4) Homogenizing the emulsion prepared in the step (3) for 2 times by using a homogenizer, wherein the homogenizing pressure is 35MPa for the first time and 32MPa for the second time.
(5) And (3) pasteurizing the homogenized material in the step (4) under the pasteurization condition of 68 ℃ for 30min.
(6) Spray drying the pasteurized material at 168 ℃ and 82 ℃ to obtain the sheep-based DHA microcapsule powder.
The polyunsaturated fatty acid grease is treated by adopting a special process, and the treatment method comprises the following steps:
s1, catalyzing ethyl esterification, namely adding alkali and ethanol into polyunsaturated fatty acid glyceride with the content of 25-30%, wherein the mass ratio of the ethanol to the polyunsaturated fatty acid glyceride is 1.0, and catalyzing the ethyl esterification, wherein the reaction temperature is 65-70 ℃;
s2, molecular distillation is carried out, and the distillation temperature is 100-110 ℃;
s3, transesterification, namely adding lipase into the distilled polyunsaturated fatty acid glyceride, wherein the transesterification temperature is 50-60 ℃;
s4, performing secondary molecular distillation at the temperature of 215-255 ℃ to obtain unsaturated fatty glyceride with the content of 40-50%.
And (2) carrying out low-temperature short-time deodorization on the unsaturated fatty glyceride with the content of 40-50% obtained in the step (S4), wherein the deodorization condition is that the temperature is 170 ℃, the time is 45-65 min, and the residual pressure is high: 230 to 235Pa, adding nitrogen into the deodorized polyunsaturated fatty acid glyceride, and then adding citric acid and an oil-soluble antioxidant.
The detection shows that the peroxide value of the surface oil is 0.14%, and the anisole value is 0.1 after 46 days of destructive test at 60 ℃ and 1.5 mmol/kg.
Example 3
In this example, the method for preparing stabilized Yang Ji ARA (or DHA) microcapsule powder comprises the steps of:
(1) Preparing an aqueous phase: weighing 19kg of wall material sheep concentrated whey protein powder and 50.9kg of solid corn syrup, weighing 3.8kg of aqueous antioxidant sodium ascorbate, weighing 0.1kg of aqueous emulsifier mono-diglycerol fatty acid ester, weighing 10g of acidity regulator sodium citrate, dissolving in pure water of 150kg at 65 ℃, and stirring until complete dissolution.
(2) Preparing an oil phase: 24kg of ARA (or DHA) grease which is a core material treated by a special process, 2kg of sunflower seed oil, 105.6g of ascorbyl palmitate which is an oil phase antioxidant, 19.2g of vitamin E and 36g of phospholipid which is an oil phase emulsifier are weighed and uniformly mixed.
(3) Adding the oil phase prepared in the step (2) into the water phase prepared in the step (1), and pre-homogenizing by using a shearing machine to obtain an emulsion.
(4) Homogenizing the emulsion prepared in the step (3) for 2 times by using a homogenizer, wherein the first homogenizing pressure is 33MPa, and the second homogenizing pressure is 30MPa.
(5) And (3) pasteurizing the homogenized material in the step (4) under the pasteurization condition of 68 ℃ for 30min.
(6) Spray drying the pasteurized material at 168 deg.C and 82 deg.C to obtain sheep-based ARA (or DHA) microcapsule powder.
The polyunsaturated fatty acid grease is treated by adopting a special process, and the treatment method comprises the following steps:
s1, catalyzing ethyl esterification, namely adding alkali and ethanol into polyunsaturated fatty acid glyceride with the content of 25-30%, wherein the mass ratio of the ethanol to the polyunsaturated fatty acid glyceride is 1.2, and catalyzing the ethyl esterification, wherein the reaction temperature is 65-70 ℃;
s2, molecular distillation is carried out, and the distillation temperature is 100-110 ℃;
s3, transesterification, namely adding lipase into the distilled polyunsaturated fatty acid glyceride, wherein the transesterification temperature is 50-60 ℃;
s4, performing secondary molecular distillation at the temperature of 215-255 ℃ to obtain unsaturated fatty glyceride with the content of 40-50%.
And (2) carrying out low-temperature short-time deodorization on the unsaturated fatty glyceride with the content of 40-50% obtained in the step (S4), wherein the deodorization condition is that the temperature is 170 ℃, the time is 45-65 min, and the residual pressure is high: 230 to 235Pa, adding nitrogen into the deodorized polyunsaturated fatty acid glyceride, and then adding citric acid and an oil-soluble antioxidant.
The detected peroxide value of the surface oil is 0.12 or 0.10 percent, and the peroxide value of the destructive test at 60 ℃ on 46 th day is 1.79 or 2.04mmol/kg, and the anisole value is 0.1.
Comparative example 1
This comparative example is essentially identical to the preparation of example 1, the most critical differences being only that: in this comparative example, the core material, which is the main component of the oil phase employed in step (2), was not subjected to a special process.
The finished microcapsule powder thus obtained was tested for surface oil of 0.17%, and after 46 days of destructive testing at 60℃the peroxide value was 5.4meq/kg, the anisidine value was 3.2 (a peroxide value exceeding 5meq/kg is unacceptable, indicating that the product processed in comparative example 1 was not sufficiently stable, and the anisidine value was 30 times higher than in example 1).
Comparative example 2
This comparative example is essentially identical to the preparation of example 2, the most critical differences being only that: in this comparative example, the sodium ascorbate fraction used in step (1) was only 0.5%.
The finished microcapsule powder thus obtained was tested for surface oil of 0.21% and, after 46 days of the 60℃destructive test, had a peroxide number of 5.7meq/kg and an anisidine number of 1.1 (a peroxide number exceeding 5meq/kg being unacceptable, indicates that the product processed in comparative example 2 is not sufficiently stable and that the anisidine number is 10 times higher than in example 2).
Comparative example 3
This comparative example is essentially identical to the preparation of example 3, the most critical differences being only that: in the comparative example, the main component of the oil phase adopted in the step (2), i.e., the core material, is not subjected to special process treatment and sunflower seed oil with good oxidation resistance is not added in the preparation of the oil phase in the step (2) to enhance the stability of the oil phase again.
The finished microcapsule powder thus obtained was tested for 0.10% or 0.09% surface oil, a peroxide number of 5.2 or 5.4meq/kg after 46 days of the 60℃destructive test, and an anisidine number of 1.6 or 1.9 (a peroxide number exceeding 5meq/kg being unacceptable, indicating that the product processed in comparative example 3 is not sufficiently stable, an anisidine number of 10 times higher than that in example 3).
Many specific embodiments of the invention are described above as merely preferred embodiments of the invention. Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown, it is well suited to various fields of use and further modifications may be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and embodiments shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (15)
1. A stabilized sheep-based unsaturated fatty acid grease microcapsule powder which is characterized in that: comprises the following components in percentage by mass:
40.91 to 92.5 percent of wall material;
5% -50% of core material;
2.5 to 8 percent of antioxidant;
0 to 0.99 percent of emulsifying agent;
0 to 0.1 percent of acidity regulator;
the wall material comprises sheep-derived proteins and plant-derived carbohydrates;
the core material comprises processed polyunsaturated fatty acid grease or processed polyunsaturated fatty acid grease blended by sunflower seed oil;
the antioxidants include aqueous phase antioxidants and oil phase antioxidants;
the emulsifier comprises an aqueous phase emulsifier and an oil phase emulsifier.
2. The stabilized sheep-based unsaturated fatty acid lipid microcapsule powder according to claim 1, wherein: the polyunsaturated fatty acid grease, namely the core material, is prepared by the following steps:
s1, catalyzing ethyl esterification, namely adding alkali and ethanol into polyunsaturated fatty acid glyceride with the content of 25-30%, wherein the mass ratio of the ethanol to the polyunsaturated fatty acid glyceride is 1.0-1.2, and catalyzing the ethyl esterification, wherein the reaction temperature is 65-70 ℃;
s2, molecular distillation is carried out, and the distillation temperature is 100-110 ℃;
s3, transesterification, namely adding lipase into the distilled polyunsaturated fatty acid glyceride, wherein the transesterification temperature is 50-60 ℃;
s4, performing secondary molecular distillation at the temperature of 215-255 ℃ to obtain unsaturated fatty glyceride with the content of 40-50%.
3. The stabilized sheep-based unsaturated fatty acid lipid microcapsule powder according to claim 2, wherein: and (2) carrying out low-temperature short-time deodorization on the unsaturated fatty glyceride with the content of 40-50% obtained in the step (S4), wherein the deodorization condition is that the temperature is 170 ℃, the time is 45-65 min, and the residual pressure is high: 230 to 235Pa, adding a chelating agent and an oil-soluble antioxidant into the deodorized polyunsaturated fatty acid glyceride after filling nitrogen.
4. A stabilized sheep-based unsaturated fatty acid lipid microcapsule powder according to claim 3, characterized in that: the chelating agent is citric acid.
5. The stabilized sheep-based unsaturated fatty acid lipid microcapsule powder according to claim 1, wherein: the sheep-derived protein is one or more of defatted sheep milk powder, sheep concentrated whey protein, sheep isolated whey protein, sheep casein, and sheep desalted whey powder.
6. The stabilized sheep-based unsaturated fatty acid lipid microcapsule powder according to claim 1, wherein: the plant-derived carbohydrate is selected from one or two of maltodextrin, maltose, solid corn syrup and goat lactose.
7. The stabilized sheep-based unsaturated fatty acid lipid microcapsule powder according to claim 1, wherein: the core material is one or a mixture of more than one of DHA grease, ARA grease and sunflower seed oil.
8. The stabilized sheep-based unsaturated fatty acid lipid microcapsule powder according to claim 1, wherein: the water phase antioxidant is sodium ascorbate; the oil phase antioxidant is one or two of ascorbyl palmitate, vitamin E and phospholipid.
9. The stabilized sheep-based unsaturated fatty acid lipid microcapsule powder according to claim 1, wherein: the water phase emulsifier is one or two of fatty acid ester of mono-diglycerol and fatty acid glyceride of citric acid; the oil phase emulsifier is phospholipid.
10. The stabilized sheep-based unsaturated fatty acid lipid microcapsule powder according to claim 1, wherein: the acidity regulator is one or two of citric acid, sodium citrate, dipotassium hydrogen phosphate, disodium hydrogen phosphate and sodium dihydrogen phosphate.
11. A method for preparing the stabilized sheep-based unsaturated fatty acid grease microcapsule powder according to claim 1, which is characterized in that: the preparation method comprises the following steps:
(1) Preparing an aqueous phase: weighing wall material, water phase antioxidant, water phase emulsifier and acidity regulator, dissolving in pure water at 50-65 deg.c, stirring to mix completely;
(2) Preparing an oil phase: weighing core materials, thawing in water bath, and adding oil phase antioxidant, wherein the oil phase emulsifier is contained, mixing uniformly, shearing for 1-30 min by using a high-efficiency shearing machine until the temperature of the oil phase rises to 1-5 ℃;
(3) Pumping the oil phase prepared in the step (2) into the water phase prepared in the step (1), and pre-homogenizing by using a high-speed shearing machine to disperse the oil phase in the water phase to form emulsion;
(4) Homogenizing the emulsion prepared in the step (3) for 1-2 times;
(5) Pasteurizing or high-temperature instantaneous sterilizing the homogenized emulsion in the step (4);
(6) And (3) carrying out spray drying on the feed liquid in the step (5) to obtain the stabilized sheep-based unsaturated fatty acid grease microcapsule powder.
12. The method for preparing the stabilized sheep-based unsaturated fatty acid grease microcapsule powder according to claim 10, which is characterized in that: in the step (1), the weight of the pure water is 1 to 1.6 times of the total weight of the microcapsule powder.
13. The method for preparing the stabilized sheep-based unsaturated fatty acid grease microcapsule powder according to claim 10, which is characterized in that: in the step (4), the homogenizing pressure is 25-45 MPa, and the second homogenizing pressure can be equal to or slightly lower than the first homogenizing pressure when the material is homogenized.
14. The method for preparing the stabilized sheep-based unsaturated fatty acid grease microcapsule powder according to claim 10, which is characterized in that: in the step (5), the pasteurization temperature is 60-70 ℃, the pasteurization time is 30-35 min or 80 ℃ and 15-30S are sterilized instantaneously.
15. The method for preparing the stabilized sheep-based unsaturated fatty acid grease microcapsule powder according to claim 10, which is characterized in that: in the step (6), the air inlet temperature adopted by the spray drying is 160-180 ℃ and the air outlet temperature is 70-90 ℃.
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2023
- 2023-09-13 CN CN202311180083.2A patent/CN117137143A/en active Pending
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