CN115299498A - Preparation method of high-stability OPL microcapsule powder for infant formula powder - Google Patents
Preparation method of high-stability OPL microcapsule powder for infant formula powder Download PDFInfo
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- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
- A23C9/00—Milk preparations; Milk powder or milk powder preparations
- A23C9/16—Agglomerating or granulating milk powder; Making instant milk powder; Products obtained thereby
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
- A23C9/00—Milk preparations; Milk powder or milk powder preparations
- A23C9/152—Milk preparations; Milk powder or milk powder preparations containing additives
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
- A23C9/00—Milk preparations; Milk powder or milk powder preparations
- A23C9/152—Milk preparations; Milk powder or milk powder preparations containing additives
- A23C9/1526—Amino acids; Peptides; Protein hydrolysates; Nucleic acids; Derivatives thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
- A23C9/00—Milk preparations; Milk powder or milk powder preparations
- A23C9/152—Milk preparations; Milk powder or milk powder preparations containing additives
- A23C9/1528—Fatty acids; Mono- or diglycerides; Petroleum jelly; Paraffine; Phospholipids; Derivatives thereof
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
- A23C9/00—Milk preparations; Milk powder or milk powder preparations
- A23C9/152—Milk preparations; Milk powder or milk powder preparations containing additives
- A23C9/158—Milk preparations; Milk powder or milk powder preparations containing additives containing vitamins or antibiotics
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
- A23C9/00—Milk preparations; Milk powder or milk powder preparations
- A23C9/20—Dietetic milk products not covered by groups A23C9/12 - A23C9/18
- A23C9/203—Dietetic milk products not covered by groups A23C9/12 - A23C9/18 containing bifidus-active substances, e.g. lactulose; containing oligosaccharides
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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
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
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Abstract
The invention provides a preparation method of high-stability OPL microcapsule powder for infant formula milk powder, which comprises the following steps: emulsifying OPL structure fat by an oil phase emulsifier, adding into a wall material solution consisting of egg yolk lecithin and fructo-oligosaccharide, stirring and mixing uniformly, and performing high-speed shearing and high-pressure homogenization to obtain a primary emulsion; dispersing sodium caseinate, whey protein, maltodextrin and vitamin C in water, mixing with the primary emulsion, adjusting pH, shearing at high speed, homogenizing under high pressure to obtain double-layer emulsion, and spray drying to obtain microcapsule powder. The invention combines the layer-layer self-assembly technology and the spray drying technology, and the prepared microcapsule powder contains OPL structural grease which is close to the space structure of fatty acid of Chinese breast milk. The prepared microcapsule powder obviously improves the oxidation stability of the OPL structural fat, the particle size of the powder can reach below 5 mu m, the embedding rate can be improved to 96.4 percent, and the microcapsule powder has high stability and is suitable for the production of various infant formula milk powders.
Description
Technical Field
The invention belongs to the technical field of microcapsule embedding processing, and particularly relates to a preparation method of high-stability OPL microcapsule powder for infant formula milk powder.
Background
Breast milk is a very complex and delicate nutritional system, recognized as the best food for infants, rich in a variety of nutrients, and its fat component, also known as human milk fat, is mainly composed of triglycerides (TAG, about 98%), phospholipids, and the like. TAG of human milk fat has special structural features, unsaturated fatty acids (U, such as oleic acid and linoleic acid) are mainly distributed at sn-1,3 position, while saturated fatty acids (S, mainly palmitic acid) are mainly distributed at sn-2 position. Thus, TAGs in human milk fat are of the main type with the USU structure, such as 1, 3-dioleoyl-2-palmitoyl triglyceride (OPO) and 1-oleic-2-palmitic-3-linoleic triglyceride (OPL).
Relevant research shows that OPO structure fat is closest to human milk fat structure and can better provide nutrition for infants. Based on the conclusion, domestic and foreign scholars research and produce OPO. However, in recent years, researchers have conducted more intensive studies on the TAG composition of human milk fat. As a result, contrary to some reports in Europe, the highest content of triglyceride in Chinese milk is OPL, which may be related to the difference in environment and dietary habits of Chinese lactates, for example, chinese lactates often eat higher linoleic acid vegetable oils (such as soybean oil). Therefore, in the infant formula milk powder in the Chinese market, a proper amount of OPL needs to be added to meet the nutritional requirements of infants in China. The OPL structure fat is rich in various monounsaturated fatty acids and polyunsaturated fatty acids, has volatility, is sensitive to light and heat, and limits practical production application. Application No. 202110202904.2, an infant formula milk powder rich in structural fat OPL and its preparation method, discloses an infant formula milk powder rich in structural fat OPL and mixed oil (including one or more of palm kernel oil, sunflower seed oil, soybean oil and coconut oil), but because OPL structural fat and other vegetable oil contain many unsaturated fatty acids, it is very easy to oxidize in the course of production and processing, and the physical and chemical properties of the product are relatively unstable. Application number 201310381604.0 'preparation method of OPO structure grease powder' discloses a preparation method of OPO structure grease microcapsule powder, wherein the stability of OPO is improved through an embedding technology, and targeted release is controlled, so that the application market is expanded. However, the research and production at present have not focused on OPL structural lipids and their embedding technology, which are more suitable for infants in china. Therefore, the microcapsule technology can be used for embedding OPL to prepare OPL structure lipid microcapsule powder, so that the OPL structure lipid is more stable in storage and use, and better provides nutrition for the growth and development of Chinese infants.
Among numerous microencapsulation methods, the spray drying method is widely applied at present because of its mature process and low operation cost. However, when the spray drying method is adopted to prepare the microcapsule, the solvent is evaporated at instantaneous high temperature, so that the wall capsule of the microcapsule is easy to crack, and the compactness can not be ensured. Therefore, the invention combines the layer-layer self-assembly technology with the spray drying to prepare the microcapsule, aiming at preparing the OPL microcapsule powder with high stability. The layer-layer self-assembly method is characterized in that a double-layer emulsion with complete structure and stable performance is formed between layers by virtue of the electrostatic attraction between egg yolk lecithin and sodium caseinate. The structure, the shape and the size of the microcapsule can be accurately controlled by combining the two methods.
Therefore, the high-stability OPL microcapsule powder for preparing the milk powder for the infants is prepared for the infants in China, and is beneficial to improving the calcium absorption of the infants, reducing the loss of calcium in excrement, reducing constipation and difficult defecation, improving the absorption and utilization of fat and promoting the growth and development of the bones of the infants.
Disclosure of Invention
The technical problem to be solved is as follows: the invention provides a preparation method of high-stability OPL structure fat microcapsule powder in order to overcome the defects that OPL structure fat is easy to be oxidized and decomposed in infant formula milk powder and a small intestine targeted controlled release system is lacked, and all the ingredients can be applied to the infant formula milk powder.
The technical scheme is as follows: a preparation method of high-stability OPL microcapsule powder for infant formula powder comprises the following steps:
(1) Heating the OPL structural grease to 45-60 ℃ for melting, and adding an oil phase emulsifier to prepare an emulsified core material;
(2) Adding fructo-oligosaccharide into water to obtain fructo-oligosaccharide aqueous solution, adding egg yolk lecithin, stirring to disperse uniformly to obtain single-layer wall material solution;
(3) Uniformly dispersing the emulsified core material and single-layer wall material solution according to the mass ratio of (2;
(4) Adding water to dissolve sodium caseinate, whey protein, maltodextrin and vitamin C according to a certain mass ratio to prepare a double-layer wall material solution;
(5) Adding the OPL structure lipid single-layer emulsion into a double-layer wall material solution according to a certain solid mass ratio, adjusting the pH to 3.5-4, shearing at a high speed, and homogenizing at a high pressure to prepare the OPL structure lipid double-layer emulsion;
(6) And (3) carrying out spray drying on the OPL structure lipid double-layer emulsion to obtain OPL microcapsule powder.
In one embodiment of the present invention, the oil phase emulsifier in step (1) is preferably lauric acid monoglyceride or citric acid fatty acid glyceride, and the mass ratio is 0.5% to 1.5%, preferably 1%, of the OPL structured fat; GB2760-2014 states that both emulsifiers can be used in infant formulas. Wherein the citric acid fatty acid glycerate has emulsifying, antioxidant, synergistic, and fat aggregation controlling effects. The lauric acid monoglyceride is an excellent emulsifier, is a safe, efficient and broad-spectrum antibacterial agent, is not limited by pH, and still has a good antibacterial effect under a neutral or slightly alkaline condition. Furthermore, lauric acid (C12: 0) accounts for about 3% of the fatty acid composition of breast milk, and lauric acid can be supplemented by adding lauric monoglyceride.
In one embodiment of the present invention, the mass ratio of the fructo-oligosaccharide to the egg yolk lecithin in step (2) is 20; the purity of the yolk lecithin is more than or equal to 80 percent of PC. GB2760-2014 stipulates that phospholipid can be added into infant formula food according to production requirements, and has certain safety. The egg yolk lecithin used as the wall material not only has emulsifying property and oxidation resistance, but also can provide sphingomyelin which does not exist in plant source lecithin, and the phospholipid composition is close to the phospholipid component in breast milk, thereby promoting the growth and development of infants.
In one embodiment of the present invention, the mass ratio of the emulsified core material and the single-layer wall material solution in step (3) is (6.
In one embodiment of the invention, the high-speed shearing rotation speed in the step (3) is 10000-13000 r/min, and the time is 1-5 min, preferably 1.5-3 min; the high-pressure homogenizing pressure is preferably 70-80 MPa, and the circulation is performed for 1-2 times.
In one embodiment of the present invention, the solid-solid ratio of the bilayer wall material solution in the step (4) is preferably: sodium caseinate whey protein maltodextrin vitamin C = 0.5; the sodium caseinate and the whey protein in the double-layer wall material solution C can promote the formation of emulsion, reduce the interfacial tension and form a protective film, and the addition amount of the sodium caseinate and the whey protein in the invention conforms to the regulation of GB 2760-2014. In addition, the maltodextrin has wide source and low price and can assist in forming films. The vitamin C is used as antioxidant, and is beneficial to improving the immunity of the organism.
In one embodiment of the invention, the high-speed shearing rotation speed in the step (5) is 10000-13000 r/min, and the time is 1-5 min, preferably 1.5-3 min; the high-pressure homogenizing pressure is preferably 20-30 MPa, and the circulation is performed for 3-4 times.
In one embodiment of the present invention, the solid matter ratio in step (5) is: the mass ratio of the OPL-structured lipid monolayer emulsion to the double-wall material solution is (2.5.
In one embodiment of the present invention, the acidity regulator used for adjusting the pH value in step (5) is lactic acid or citric acid, which can be used in appropriate amounts according to production requirements in infant formula according to GB 2760-2014.
In one embodiment of the present invention, the temperature of the inlet air for spray drying in step (6) is preferably 170 to 180 ℃, and the flow rate is preferably 500 to 600mL/h.
The method of the invention uses egg yolk lecithin as an anionic surfactant to prepare single-layer emulsion with negatively charged droplets; the sodium caseinate is positively charged when the pH value is lower than the isoelectric point, so that a stable and firm double-layer membrane structure can be formed on the surface of the OPL structure-embedded lipid by electrostatic interaction and a high-speed shearing and high-pressure homogenizing method, and finally, the high-stability OPL microcapsule powder is prepared by spray drying.
Has the advantages that:
1. the OPL structure fat used by the method is breast milk substitute fat, and is closer to the composition of Chinese breast milk fat. The product can be applied to infant formula milk powder to improve the absorption rate of infant to fatty acid and calcium ion. The selected oil phase emulsifier is lauric acid monoglyceride or citric acid fatty acid glyceride, wherein the lauric acid monoglyceride can be used as a bactericide and provides a lauric acid component in the breast milk, and the emulsifier is a safe emulsifier which meets the national standard of infant formula.
2. The phospholipid composition of the wall material egg yolk lecithin used by the method is close to that of breast milk phospholipid, and the egg yolk lecithin has hydrophilic lipophilicity, can lead the core material in the egg yolk lecithin to be released in a targeted way, and improves the bioavailability. The selected other wall material components, such as sodium caseinate, whey protein, fructo-oligosaccharide, maltodextrin and vitamin C can be used in infant formula food, meet the national standard and have beneficial effects on the growth and development of infants.
3. The method combines a layer-layer self-assembly technology with a spray drying technology, and generates electrostatic interaction between microcapsule wall materials by adjusting pH to prepare the OPL microcapsule powder, wherein the wall materials contain two antioxidants of vitamin C and egg yolk lecithin, and the prepared OPL microcapsule powder has high embedding rate and high stability, so that the nutritive value of the OPL microcapsule powder is furthest reserved during storage, and the storage performance of the OPL microcapsule powder can be improved.
Drawings
FIG. 1 is a specific implementation process flow of high-stability OPL microcapsule powder which can be used for infant formula powder;
FIG. 2 is an appearance state of OPL-structured lipid microcapsule powder, in which (left) is a single-layer OPL-structured lipid microcapsule of comparative example 1 and (right) is a double-layer OPL-structured lipid microcapsule of example 2;
fig. 3 is a microstructure of OPL structured lipid microcapsule powder under biological scanning electron microscope, wherein: a, B and C are single-layer OPL structural lipid microcapsules (comparative example 1), and the scanning electron microscope multiples are 150X, 750X and 2000X in sequence; d, E and F are double-layer OPL structure lipid microcapsules (example 2), and the scanning electron microscope multiples are 750 times, 2000 times and 6000 times in sequence.
Detailed Description
The invention provides a preparation method of high-stability OPL microcapsule powder for preparing milk powder for infants, and in order to make the purpose, technical scheme and effect of the invention clearer and clearer, the invention is further described in detail with the aid of examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
(1) Preparation of a core material: weighing 3.30g of OPL structure fat, melting in a constant-temperature water bath at 45 ℃, uniformly stirring, adding 0.03g of lauric acid monoglyceride, stirring to dissolve the lauric acid monoglyceride in the OPL structure fat to obtain a core material, and standing for later use;
(2) Preparation of monolayer wall material solution: weighing 0.42g of egg yolk lecithin and 6.25g of fructo-oligosaccharide, adding into 37.5mL of distilled water, uniformly dispersing in the water to obtain a single-layer wall material solution, and standing for later use;
(3) Preparation of OPL structure lipid monolayer emulsion: adding the core material into the monolayer wall material solution, uniformly stirring in a constant-temperature water bath at 45 ℃, shearing at a high speed of 10000r/min for 2min, homogenizing at a high pressure of 80MPa, circulating for 1 time to obtain an OPL structure lipid monolayer emulsion, and placing for later use;
(4) Preparing a double-layer wall material solution: weighing 0.10g of sodium caseinate, 14.00g of maltodextrin, 5.80g of whey protein and 0.10g of vitamin C, adding into 112.5mL of water, dissolving and uniformly stirring to obtain a double-layer wall material solution;
(5) Preparation of OPL structure lipid bilayer emulsion: adding the OPL structure lipid single-layer emulsion into the double-layer wall material solution, adjusting the pH to 3.5, uniformly stirring in a 45 ℃ constant-temperature water bath, shearing at a high speed of 10000r/min for 2min, homogenizing at a high pressure of 20MPa, and circulating for 4 times to obtain the OPL structure lipid double-layer emulsion, and standing for later use;
(6) Preparation of OPL structured lipid microcapsule powder: and (3) carrying out spray drying on the OPL structure lipid double-layer emulsion at the inlet temperature of 170 ℃ and the flow rate of 500mL/h to obtain OPL structure lipid microcapsule powder.
Surface oil and embedding rate measurement results: the surface oil of the obtained OPL structured fat microcapsule powder was 0.0048g/0.5g microcapsule, and the entrapment rate was 91.3%.
Example 2
(1) Preparation of a core material: weighing 3.30g of OPL structure fat, melting in a constant-temperature water bath at 45 ℃, uniformly stirring, adding 0.03g of lauric acid monoglyceride, stirring to dissolve the lauric acid monoglyceride in the OPL structure fat to obtain a core material, and standing for later use;
(2) Preparation of monolayer wall material solution: weighing 0.50g of egg yolk lecithin and 7.50g of fructo-oligosaccharide, adding into 45.0mL of distilled water, uniformly dispersing in the water to obtain a single-layer wall material solution, and standing for later use;
(3) Preparation of OPL structure lipid monolayer emulsion: adding the core material A into the single-layer wall material solution, uniformly stirring in a constant-temperature water bath at 45 ℃, shearing at a high speed of 10000r/min for 2min, homogenizing at a high pressure of 80MPa, circulating for 1 time to obtain an OPL structure lipid single-layer emulsion, and standing for later use;
(4) Preparing a double-layer wall material solution: weighing 0.09g of sodium caseinate, 13.67g of maltodextrin, 5.41g of whey protein and 0.09g of vitamin C, adding into 105.0mL of water, dissolving and uniformly stirring;
(5) Preparation of OPL structure lipid bilayer emulsion: adding the OPL structure lipid single-layer emulsion into the double-layer wall material solution, adjusting the pH to 3.5, uniformly stirring in a 45 ℃ constant-temperature water bath, shearing at a high speed of 10000r/min for 2min, homogenizing at a high pressure of 20MPa, and circulating for 4 times to obtain the OPL structure lipid double-layer emulsion, and standing for later use;
(6) Preparation of OPL structured lipid microcapsule powder: and (3) carrying out spray drying on the OPL structural lipid double-layer emulsion at the inlet temperature of 170 ℃ and the flow rate of 500mL/h to obtain OPL structural lipid microcapsule powder.
Surface oil and entrapment rate measurement results: the surface oil of the obtained OPL structured fat microcapsule powder is 0.0020g/0.5g microcapsule, and the embedding rate is 96.4%.
Example 3
(1) Preparation of a core material: weighing 3.30g of OPL structure fat, melting in a constant-temperature water bath at 45 ℃, uniformly stirring, adding 0.03g of lauric acid monoglyceride, stirring to dissolve the lauric acid monoglyceride in the OPL structure fat to obtain a core material, and standing for later use;
(2) Preparation of monolayer wall material solution: weighing 0.58g of egg yolk lecithin and 8.75g of fructo-oligosaccharide into 52.5mL of distilled water, uniformly dispersing the egg yolk lecithin and the fructo-oligosaccharide in the distilled water to obtain a single-layer wall material solution, and standing for later use;
(3) Preparation of OPL structure lipid monolayer emulsion: adding the core material into the monolayer wall material solution, uniformly stirring in a constant-temperature water bath at 45 ℃, shearing at a high speed of 10000r/min for 2min, homogenizing at a high pressure of 80MPa, circulating for 1 time to obtain an OPL structure lipid monolayer emulsion, and placing for later use;
(4) Preparing a double-layer wall material solution: weighing 0.09g of sodium caseinate, 12.13g of maltodextrin, 5.03g of whey protein and 0.09g of vitamin C, adding the mixture into 97.5mL of water, dissolving and uniformly stirring;
(5) Preparation of OPL structure lipid bilayer emulsion: adding the OPL structural lipid monolayer emulsion into the double-layer wall material solution, adjusting the pH to 3.5, uniformly stirring in a constant-temperature water bath at 45 ℃, shearing at a high speed of 10000r/min for 2min, homogenizing at a high pressure of 20MPa, and circulating for 4 times to obtain the OPL structural lipid monolayer emulsion, and standing for later use;
(6) Preparation of OPL structured lipid microcapsule powder: and (3) carrying out spray drying on the OPL structure lipid double-layer emulsion at the inlet temperature of 170 ℃ and the flow rate of 500mL/h to obtain OPL structure lipid microcapsule powder.
Surface oil and embedding rate measurement results: the surface oil of the obtained OPL structured fat microcapsule powder was 0.0037g/0.5g microcapsule, and the entrapment rate was 93.3%.
Example 4
(1) Preparing a core material: weighing 3.30g of OPL structure fat, melting in a constant-temperature water bath at 45 ℃, uniformly stirring, adding 0.03g of lauric acid monoglyceride, stirring to dissolve the lauric acid monoglyceride in the OPL structure fat to obtain a core material, and standing for later use;
(2) Preparation of monolayer wall material solution: weighing 0.67g of egg yolk lecithin and 10.00g of fructo-oligosaccharide, adding into 60.0mL of distilled water, uniformly dispersing in the water to obtain a single-layer wall material solution, and standing for later use;
(3) Preparation of OPL structure lipid monolayer emulsion: adding the core material into the single-layer wall material solution, uniformly stirring in a constant-temperature water bath at 45 ℃, shearing at a high speed of 10000r/min for 2min, homogenizing at a high pressure of 80MPa, circulating for 1 time to obtain an OPL structure lipid single-layer emulsion, and standing for later use;
(4) Preparing a double-layer wall material solution: weighing 0.08g of sodium caseinate, 11.20g of maltodextrin, 4.64g of whey protein and 0.08g of vitamin C, adding into 90.0mL of water, dissolving and uniformly stirring;
(5) Preparation of OPL structure lipid bilayer emulsion: adding the OPL structure lipid single-layer emulsion into the double-layer wall material solution, adjusting the pH to 3.5, uniformly stirring in a 45 ℃ constant-temperature water bath, shearing at a high speed of 10000r/min for 2min, homogenizing at a high pressure of 20MPa, and circulating for 4 times to obtain the OPL structure lipid double-layer emulsion, and standing for later use;
(6) Preparation of OPL structured lipid microcapsule powder: and (3) carrying out spray drying on the OPL structure lipid double-layer emulsion at the inlet temperature of 170 ℃ and the flow rate of 500mL/h to obtain OPL structure lipid microcapsule powder.
Surface oil and entrapment rate measurement results: the surface oil of the obtained OPL structured fat microcapsule powder was 0.0049g/0.5g microcapsule, and the entrapment rate was 91.1%.
Example 5
(1) Preparation of a core material: weighing 3.30g of OPL structure fat, melting in a constant-temperature water bath at 45 ℃, uniformly stirring, adding 0.03g of lauric acid monoglyceride, stirring to dissolve the lauric acid monoglyceride in the OPL structure fat to obtain a core material, and standing for later use;
(2) Preparation of monolayer wall material solution: weighing 0.75g of egg yolk lecithin and 11.25g of fructo-oligosaccharide, adding into 67.5mL of distilled water, uniformly dispersing in the water to obtain a single-layer wall material solution, and standing for later use;
(3) Preparation of OPL structure lipid monolayer emulsion: adding the core material into the single-layer wall material solution, uniformly stirring in a constant-temperature water bath at 45 ℃, shearing at a high speed of 10000r/min for 2min, homogenizing at a high pressure of 80MPa, circulating for 1 time to obtain an OPL structure lipid single-layer emulsion, and standing for later use;
(4) Preparing a double-layer wall material solution: weighing 0.07g of sodium caseinate, 10.27g of maltodextrin, 4.25g of whey protein and 0.07g of vitamin C, adding into 82.5mL of water, dissolving and uniformly stirring;
(5) Preparation of OPL structure lipid bilayer emulsion: adding the OPL structural lipid monolayer emulsion into the double-layer wall material solution C, adjusting the pH to 3.5, uniformly stirring in a constant-temperature water bath at 45 ℃, shearing at a high speed of 10000r/min for 2min, homogenizing at a high pressure of 20MPa, and circulating for 4 times to obtain the OPL structural lipid monolayer emulsion, and standing for later use;
(6) Preparation of OPL structured lipid microcapsule powder: and (3) carrying out spray drying on the OPL structural lipid double-layer emulsion at the inlet temperature of 170 ℃ and the flow rate of 500mL/h to obtain OPL structural lipid microcapsule powder.
Surface oil and embedding rate measurement results: the surface oil of the obtained OPL structured fat microcapsule powder was 0.0059g/0.5g microcapsule, and the entrapment rate was 89.3%.
The microcapsules prepared in examples 1 to 5 were examined and compared, and table 1 shows the physical and chemical properties of the OPL-structured lipid microcapsule powder, and table 2 shows the microbial indicators of the OPL-structured lipid microcapsule powder.
Comparative example 1
The difference between the preparation method of the comparative example and the preparation method of the embodiment is that the OPL structure lipid monolayer emulsion is directly subjected to spray drying after being prepared, and the obtained product is OPL structure lipid monolayer microcapsule powder.
The embedding rate of the OPL single-layer microcapsule powder prepared by the method is 76.2%, the color gradually turns yellow and the oxidation degree is increased in the process of accelerated storage at 60 ℃ for 20 days, and the peroxidation value is 25.6meq/kg after 20 days, and the analysis reason is probably that the single-layer structure cannot protect the OPL structural grease of the core material for a long time.
Comparative example 2
The comparative example is different from the preparation method of the example in that the ratio of the ingredient whey protein is changed under the premise that the solid content is constant. Preparing a double-layer wall material solution in the step (4): 0.07g of sodium caseinate, 12.52g of maltodextrin, 2g of whey protein and 0.07g of vitamin C are weighed and added into 82.5mL of water to be dissolved and stirred uniformly.
The embedding rate of the OPL microcapsule powder prepared by the method is 85%, the peroxide value is 17.8meq/kg after the OPL microcapsule powder is stored for 20 days at the temperature of 60 ℃, and the analysis reason is probably that the double-layer structure microcapsule prepared by the invention is formed by utilizing the electrostatic interaction between the negative charge of the egg yolk lecithin of the first layer and the positive charge of the whey protein of the second layer at the low pH value, so the electrostatic interaction between the double-layer structures is weakened due to the reduction of the content of the whey protein in the second layer, and the embedding rate is reduced. During storage, the OPL structural grease of the core material seeps out, the surface oil is increased, and the peroxide value is increased.
Comparative example 3
In "a method for preparing a mother emulsified nutritional oil microcapsule powder" with publication No. CN 106974267A, the difference from this example is that, when preparing a wall material solution, 63.75g of wall materials (lactose, whey protein and skim milk powder 18.
The microcapsule powder thus prepared uses a higher content of sodium caseinate and sodium starch octenyl succinate, which reaches the maximum usage of 1g/kg of sodium caseinate and sodium starch octenyl succinate in infant formula, accounting for 1% of the total solid content, specified in GB2760-2014, thereby limiting further applications of the microcapsule powder thus prepared in infant formula. The content of the sodium caseinate used as the emulsifier in the invention is only 0.23-0.33% of the total solid content, and the sodium caseinate has important application potential in infant formula foods.
TABLE 1 physicochemical Properties of OPL-structured lipid microcapsule powders
TABLE 2 microbiological index of OPL structured lipid microcapsule powder
Claims (10)
1. A preparation method of high-stability OPL microcapsule powder for infant formula milk powder is characterized by comprising the following steps:
(1) Heating OPL structure grease to 45-60 ℃ for melting, and adding an oil phase emulsifier to prepare an emulsified core material;
(2) Adding fructo-oligosaccharide into water to obtain fructo-oligosaccharide aqueous solution, adding egg yolk lecithin, stirring to disperse uniformly to obtain single-layer wall material solution;
(3) Uniformly dispersing the emulsified core material and single-layer wall material solution according to the mass ratio of (2;
(4) Adding water to dissolve sodium caseinate, whey protein, maltodextrin and vitamin C according to a certain mass ratio to prepare a double-layer wall material solution;
(5) Adding the OPL structure lipid single-layer emulsion into a double-layer wall material solution according to a certain solid mass ratio, adjusting the pH to 3.5-4, shearing at a high speed, and homogenizing at a high pressure to prepare the OPL structure lipid double-layer emulsion;
(6) And (3) carrying out spray drying on the OPL structure lipid double-layer emulsion to obtain OPL microcapsule powder.
2. The preparation method of the high-stability OPL microcapsule powder used for infant formula powder according to claim 1, characterized in that the oil phase emulsifier in step (1) is preferably lauric acid monoglyceride fatty acid ester or citric acid fatty acid glyceride, and the mass ratio is 0.5% -1.5% of OPL structural fat, preferably 1%.
3. The preparation method of the high-stability OPL microcapsule powder for the infant formula powder according to claim 1, wherein the mass ratio of the fructo-oligosaccharide to the egg yolk lecithin in the step (2) is 20 to 10, and preferably 15.
4. The preparation method of the high-stability OPL microcapsule powder for the infant formula powder according to claim 1, characterized in that the mass ratio of the emulsified core material and the single-layer wall material solution in step (3) is (6.
5. The preparation method of the high-stability OPL microcapsule powder used for infant formula powder according to claim 1, characterized in that the high-speed shearing rotation speed in step (3) is 10000-13000 r/min, the time is 1-5 min, preferably 1.5-3 min; the high-pressure homogenization pressure is preferably 70-80 MPa, and the circulation is 1-2 times.
6. The method for preparing high-stability OPL microcapsule powder for infant formula powder according to claim 1, wherein the OPL microcapsule powder comprises: the mass ratio of the solid matters of the double-layer wall material solution in the step (4) is preferably as follows: sodium caseinate whey protein maltodextrin vitamin C = 0.5.
7. The preparation method of the high-stability OPL microcapsule powder for the infant formula powder according to claim 1, characterized in that the high-speed shearing rotation speed in step (5) is 10000-13000 r/min for 1-5 min, preferably 1.5-3 min; the high-pressure homogenizing pressure is preferably 20-30 MPa, and the circulation is performed for 3-4 times.
8. The method for preparing high-stability OPL microcapsule powder used for infant formula powder according to claim 1, characterized in that: the solid substance mass ratio in the step (5) is as follows: the mass ratio of the OPL-structure lipid monolayer emulsion to the double-layer wall material solution is (2.5.
9. The method for preparing high-stability OPL microcapsule powder for infant formula powder according to claim 1, wherein the acidity regulator used for pH adjustment in step (5) is lactic acid or citric acid.
10. The preparation method of the high-stability OPL microcapsule powder for infant formula powder according to claim 1, characterized in that the air inlet temperature of the spray drying in the step (6) is preferably 170-180 ℃, and the flow rate is preferably 500-600 mL/h.
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| CN110613025A (en) * | 2019-10-11 | 2019-12-27 | 湖北欣和生物科技有限公司 | High-oil-loading microcapsule powder and preparation method thereof |
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| CN108902326A (en) * | 2018-07-23 | 2018-11-30 | 东北农业大学 | A kind of novel soybean milk powder formula |
| CN110613025A (en) * | 2019-10-11 | 2019-12-27 | 湖北欣和生物科技有限公司 | High-oil-loading microcapsule powder and preparation method thereof |
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