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CN115251363A - Nano emulsion taking milk phospholipid as emulsifier and preparation method and application thereof - Google Patents

Nano emulsion taking milk phospholipid as emulsifier and preparation method and application thereof Download PDF

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Publication number
CN115251363A
CN115251363A CN202210934416.5A CN202210934416A CN115251363A CN 115251363 A CN115251363 A CN 115251363A CN 202210934416 A CN202210934416 A CN 202210934416A CN 115251363 A CN115251363 A CN 115251363A
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emulsion
emulsifier
milk phospholipid
nano
phospholipid
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郑旭
关莹
于婷
张树刚
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Yuneng Dalian Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/10Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Colloid Chemistry (AREA)

Abstract

The invention discloses a nano emulsion taking milk phospholipid as an emulsifier, and a preparation method and application thereof. A nano-emulsion taking milk phospholipid as an emulsifier comprises the following raw materials in parts by weight: 0.1-2 parts of milk phospholipid, 1-10 parts of functional grease and 90-99 parts of water, and the preparation method comprises the following steps: s1: heating water to 50-80 deg.C, adding milk phospholipid, and mixing to obtain hydrated milk phospholipid emulsifier; s2: uniformly mixing the functional grease and the hydrated milk phospholipid emulsifier prepared in the step S1, and homogenizing for 1 time to obtain a coarse emulsion; s3: and (3) homogenizing the coarse emulsion prepared in the step (S2) for 1-3 times to obtain the nano emulsion which can be applied to food and takes the milk phospholipid as an emulsifier. The invention discloses a nano emulsion using milk phospholipid as emulsifier and a preparation method and application thereof, wherein the milk phospholipid is used for producing high temperature resistant emulsion, the particle size reaches the nano level, the Zeta potential absolute value is more than 30mV, and the high temperature resistant emulsion can keep stable at 121 ℃.

Description

Nano emulsion taking milk phospholipid as emulsifier and preparation method and application thereof
Technical Field
The invention relates to the technical field of nano-emulsion, in particular to nano-emulsion taking milk phospholipid as an emulsifier, and a preparation method and application thereof.
Background
The milk phospholipid is an easily dispersible, high temperature resistant emulsifier, and has double functions of nutrition and emulsification. Milk phospholipids are a good source of sphingomyelin, gangliosides and ceramides. Milk phospholipids have a pure milk taste and flavor relative to common soy phospholipids. Milk phospholipids can improve intestinal health, contribute to gut maturation and immune system stabilization. The phospholipid serine in milk phospholipid can improve pressure, reduce memory deterioration, and is helpful for brain development of infants.
In recent years, food-grade nano emulsion as a simple and effective embedding and transporting system is widely applied to embedding and transferring functional grease and various oil-soluble nutrients, can prevent functional nutrient components from being oxidized, and improves the water solubility and bioavailability of the functional nutrient components. The nano emulsion is also different from the common emulsion in that the nano emulsion can resist flocculation, coalescence and gravity separation in the storage process and is a near-thermodynamic stable system. The preparation method of the nano emulsion comprises a high-energy method and a low-energy method, and the high-pressure homogeneous emulsification technology is used as a commonly used high-energy method for preparing the nano emulsion and has the advantages of small emulsion particle size, uniform distribution, stable emulsion system, small demand of a surfactant and the like.
Patent CN106723052A discloses a preparation method of omega-3 rich linseed oil nanoemulsion, which prepares nanoemulsion by high-pressure homogenization method. Patent CN109122905A discloses a preparation method of sea buckthorn oil nano-emulsion and sea buckthorn oil nano-emulsion, which is prepared by adopting sodium caseinate emulsifier through high-pressure homogenization, wherein the nano-emulsion reported in the two patents contains a high-content emulsifier, and the soy lecithin has poor flavor at high temperature, and the protein emulsifier gradually loses activity at the temperature of more than 80-90 ℃, so that the nano-emulsion has poor thermal stability and cannot adapt to the high-temperature condition of 121 ℃.
Disclosure of Invention
The invention discloses a nano emulsion using milk phospholipid as emulsifier and a preparation method and application thereof, wherein the milk phospholipid is used for producing high temperature resistant emulsion, the particle size reaches the nano level, the Zeta potential absolute value is more than 30mV, and the high temperature resistant emulsion can keep stable at 121 ℃.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a nano-emulsion taking milk phospholipid as an emulsifier comprises the following raw materials in parts by weight: 0.1-2 parts of milk phospholipid, 5 parts of functional grease and 95 parts of water.
Further, the feed additive comprises the following raw materials in parts by weight: 0.1-1 part of milk phospholipid, 1-5 parts of functional grease and 95-99 parts of water; furthermore, the feed additive is composed of the following raw materials in parts by weight: 1 part of milk phospholipid, 5 parts of functional grease and 95 parts of water.
Further, the functional grease is at least one selected from sea buckthorn oil, DHA algae oil, acer truncatum seed oil, plukenetia volubilis oil and silybum marianum oil.
Furthermore, the particle size of the nano emulsion taking the milk phospholipid as the emulsifier is 170.3-217.9nm.
The invention discloses a nano-emulsion taking milk phospholipid as an emulsifier, which has the following beneficial effects:
1. by mixing the functional grease, the milk phospholipid and the water and controlling 5 parts of the functional grease, 1 part of the milk phospholipid and 95 parts of the water, oil drops are not easy to fuse, so that the particle size of the nano emulsion is kept at a nano level.
2. The milk phospholipid is controlled to be 0.1-2 parts by weight, so that the emulsifier can completely wrap oil drops and keep stable under the high-temperature condition.
A method for preparing nano emulsion by taking milk phospholipid as an emulsifier mainly comprises the following steps:
s1: heating water to 50-80 deg.C, adding milk phospholipid, and mixing to obtain hydrated milk phospholipid emulsifier;
s2: uniformly mixing the functional grease and the hydrated milk phospholipid emulsifier prepared in the step S1, and homogenizing for 1 time in a homogenizer with the pressure of 20-40Mpa to obtain a crude emulsion;
s3: homogenizing the crude emulsion obtained in step S2 in a high pressure homogenizer with pressure of 100-150Mpa for 1-3 times to obtain nanometer emulsion with milk phospholipid as emulsifier.
Further, in the step S1, the mixing mode is mechanical stirring, the rotating speed is 800-1000r/min, and the stirring time is 10-120min.
Further, in step S3, the number of homogenization times is 2-3, and further, in step S3, the number of homogenization times is 3.
An application of nano emulsion with milk phospholipid as emulsifier in food.
The invention discloses a preparation method and application of nano emulsion taking milk phospholipid as an emulsifier, which has the following beneficial effects:
1. the problem of poor thermal stability of the nano emulsion prepared by taking protein as an emulsifier is solved by adopting the milk phospholipid to prepare the nano emulsion, and the milk phospholipid can cover the unpleasant odor of functional grease and solve the problem of poor flavor of the nano emulsion under the high-temperature condition;
2. the particle size of the nano emulsion prepared by the preparation method and taking the milk phospholipid as the emulsifier is 170.3-217.9nm, the nano emulsion can be kept stable at the high temperature of 121 ℃, the storage stability is high, the nano emulsion can be kept uniform and not layered after being placed for 30 days at the temperature of 37 ℃ and the humidity of 70 ℃;
3. the method is simple and easy to operate, and is suitable for large-scale industrial production and processing.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, comparative examples and performance test data, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The starting materials used in this application are all commercially available.
Examples
A method for preparing nano emulsion by taking milk phospholipid as an emulsifier mainly comprises the following steps:
s1: heating water to 50 ℃, adding milk phospholipid, mixing and stirring in a mechanical stirring mode at the rotating speed of 1000r/min for 60min to ensure that the milk phospholipid is fully hydrated in the water to form a hydrated milk phospholipid emulsifier;
s2: uniformly mixing the functional grease and the hydrated milk phospholipid emulsifier prepared in the step S1 in a mechanical stirring manner, and homogenizing for 1 time in a homogenizer with the pressure of 30Mpa to obtain a coarse emulsion;
s3: homogenizing the coarse emulsion obtained in step S2 in a high-pressure homogenizer with pressure of 150Mpa for 3 times to obtain the nano emulsion with milk phospholipid as emulsifier.
Table 1: EXAMPLES 1-9 raw materials and content Table (unit: g)
Figure BDA0003782894520000041
Example 10: the difference from example 1 is that in step S3, the number of homogenization times is 1.
Example 11: the difference from example 1 is that in step S3, the number of homogenization times is 2.
Example 12: the difference from example 1 is that in step S3, the homogenizing pressure is 100MPa.
Comparative example
Comparative example 1: the difference from example 1 is that in step S3, the number of homogenizations is 4.
Comparative example 2: a method for preparing nano emulsion by taking milk phospholipid as an emulsifier mainly comprises the following steps: s1: heating 80g of water to 50 ℃, adding 3g of milk phospholipid, mixing and stirring in a mechanical stirring manner at the rotating speed of 1000r/min for 60min to ensure that the milk phospholipid is fully hydrated in the water to form a hydrated milk phospholipid emulsifier;
s2: uniformly mixing 20g of sea buckthorn oil and the hydrated milk phospholipid emulsifier prepared in the step S1 in a mechanical stirring manner, and homogenizing for 1 time in a homogenizer with the pressure of 30Mpa to obtain a crude emulsion;
s3: homogenizing the coarse emulsion obtained in step S2 in a high-pressure homogenizer with pressure of 150Mpa for 3 times to obtain nanometer emulsion with milk phospholipid as emulsifier.
Comparative example 3: a method for preparing nano emulsion by taking soybean lecithin as an emulsifier mainly comprises the following steps: s1: heating water to 50 ℃, adding soybean phospholipid, mixing and stirring in a mechanical stirring mode at the rotating speed of 1000r/min for 60min to ensure that the soybean phospholipid is fully hydrated in the water to form a hydrated soybean phospholipid emulsifier;
s2: uniformly mixing 5g of sea buckthorn oil and the hydrated soybean lecithin emulsifier prepared in the step S1 in a mechanical stirring manner, and homogenizing for 1 time in a homogenizer with the pressure of 30Mpa to obtain a coarse emulsion;
s3: homogenizing the crude emulsion obtained in step S2 in a high pressure homogenizer with pressure of 150Mpa for 3 times to obtain phospholipid nanoemulsion.
Comparative example 4: the difference from example 1 is that in step S3, the homogenizing pressure is 180MPa.
Performance test
1. The following performance tests were performed on the nanoemulsions prepared in examples 1-12 and comparative examples 1-4 above:
average particle size and Zeta potential test: particle size and potential analysis is carried out by an Oumecke NS-90Z nanometer particle size and potential analyzer;
and (3) stability testing: (1) sterilizing for 15min in a vertical steam sterilizer at 121 ℃; (2) The sterilized sample is placed in a constant temperature and humidity incubator with the temperature of 37 ℃ and the humidity of 70 ℃ for 30 days to observe the properties of the emulsion, and the detection results are shown in table 2.
Table 2: test results
Test item Average particle diameter (nm) Zeta potential (mV) 121℃、15min Standing at 37 deg.C and 70 deg.C for 30 days
Example 1 186.2 -33.7 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
Example 2 191.7 -32.1 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
Example 3 189.3 -33.3 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
Example 4 190.5 -32.7 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
Example 5 191.9 -32.2 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
Example 6 170.3 -39.2 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
Example 7 194.9 -33.1 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
Example 8 178.2 -37.1 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
Example 9 285.4 -23.2 Homogeneous, non-demixing emulsion Demixing of emulsions
Example 10 232.8 -28.8 Homogeneous, non-demixing emulsion Demixing of emulsions
Example 11 217.9 -31.1 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
Example 12 229.3 -28.4 Homogeneous, non-demixing emulsion Emulsion stratification
Comparative example 1 185.8 -33.9 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
Comparative example 2 Demixing of emulsions
Comparative example 3 192.3 -32.8 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
Comparative example 4 184.5 -34.1 Homogeneous, non-demixing emulsion Homogeneous, non-demixing emulsion
2. The nano-emulsions prepared in examples 1 to 12 and comparative examples 1 to 4 were used in beverages to examine the flavors of the samples.
Sensory evaluation method: a sensory evaluation group was composed of 10 professionals (5 persons each for men and women) and the beverage was scored comprehensively from the aspect of flavor and taste. Each sample was rested for 2min and rinsed with purified water. Specific scoring criteria are shown in table 3. Each person takes 10ml of sample and drinks it, and the characteristic feature that the sample is drunk and continues to feel is called retention.
TABLE 3 beverage evaluation criteria Table
Figure BDA0003782894520000061
The score is calculated statistically, the average value of 10 professionals is taken, and the evaluation result is shown in Table 4
Figure BDA0003782894520000062
Table 4: scores for examples and comparative examples
Examples Example 1 Example 2 Example 3 Example 4 Example 5 Example 6
Score of 5.1 4.5 5.5 5.3 5.1 5.6
Examples Example 7 Example 8 Example 9 Example 10 Example 11 Example 12
Score of 5.2 5.8 3.5 3.1 4.0 3
Comparative example Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4
Score of 5.2 0.4 1.1 5.1
It can be seen from tables 2 and 4 and examples 1 to 5 that the emulsifiers in examples 1 to 5 are milk phospholipids, and the particle size and Zeta potential of the nanoemulsion prepared from sea buckthorn oil, DHA algae oil, plukenetia volubilis oil, acer truncatum seed oil and silybum marianum oil and using milk phospholipids as emulsifiers are compared. The grain diameter is not more than 200nm, and the Zeta potential absolute values are more than 30mV, so that the stability is better. Compared with 5 kinds of functional grease, the nanoemulsion taking milk phospholipid as an emulsifier prepared from the seabuckthorn oil is relatively stable from particle size and potential, and the nanoemulsion taking milk phospholipid as an emulsifier prepared from the acer truncatum seed oil has better flavor from the aspect of mouthfeel.
It can be seen from tables 2 and 4, and example 1 and comparative example 3 that the particle size of the nanoemulsion of milk phospholipid as an emulsifier is small, and the flavor of the nanoemulsion of milk phospholipid as an emulsifier after sterilization is superior to that of the nanoemulsion of soybean phospholipid as an emulsifier after sterilization.
As can be seen from Table 2 in combination with example 1, examples 10 to 11 and comparative example 1, as the number of homogenization times increases, the particle size decreases, the absolute value of Zeta potential increases, and the stability of the preparation improves. However, the results obtained by homogenizing for 4 times are slightly different from those obtained by homogenizing for 3 times, and the nanoemulsion taking milk phospholipid as an emulsifier is prepared by adopting homogenizing for 3 times in view of production efficiency.
It can be seen from Table 2, examples 1, 8-9 and comparative example to comparative example 2 that the amount of seabuckthorn oil added is different. With the increase of the seabuckthorn oil, the particle size is increased, the Zeta potential absolute value is reduced, and the stability of the nano emulsion is reduced due to the overhigh oil content.
As can be seen from the combination of Table 2 and examples 1 and 6 to 8, the particle size of the nanoemulsion decreases with a decrease in the emulsifier content, provided that the emulsion is stable.
It can be seen from table 2 and example 1, example 12 and comparative example 4 that as the homogenization pressure increases, the particle size decreases and the Zeta potential absolute value increases, improving the stability of the emulsion. As the result obtained by the homogenizing pressure of 180MPa is smaller than that obtained by the homogenizing pressure of 150MPa, the equipment loss is considered, and the nano emulsion taking the milk phospholipid as the emulsifier is prepared by adopting the homogenizing pressure of 150 MPa.
In summary, according to the present application, by mixing the functional oil, the milk phospholipid and the water, and controlling 5 parts of the functional oil, 0.1-2 parts of the milk phospholipid and 95 parts of the water, the emulsifier can completely wrap the oil droplets, and further the concentration of the emulsifier solution can be maintained within the range of 0.1wt% to 2wt%, so that the oil droplets are not easily fused, and thus the particle size of the nano emulsion reaches the nanometer level, the particle size is 170.3-217.9nm, the zeta potential absolute value is greater than 30mV, the nano emulsion can be kept stable at a high temperature of 121 ℃, the storage stability is high, and the nano emulsion can be kept uniform and not delaminated after being placed for 30 days at a temperature of 37 ℃ and a humidity of 70 °.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, those skilled in the art will appreciate that; the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (8)

1. A nano-emulsion taking milk phospholipid as an emulsifier is characterized by comprising the following raw materials in parts by weight: 0.1-2 parts of milk phospholipid, 1-10 parts of functional grease and 90-99 parts of water.
2. The nano-emulsion taking the milk phospholipid as the emulsifier according to claim 1 is characterized by comprising the following raw materials in parts by weight: 0.1-1 part of milk phospholipid, 1-5 parts of functional grease and 95-99 parts of water.
3. The nanoemulsion taking the milk phospholipid as the emulsifier according to claim 1, wherein the functional oil is at least one selected from seabuckthorn oil, DHA algae oil, acer truncatum seed oil, american vine fruit oil and silybum marianum oil.
4. The nano-emulsion taking the milk phospholipid as the emulsifier as claimed in claim 1, wherein the particle size of the nano-emulsion taking the milk phospholipid as the emulsifier is 170.3-217.9nm.
5. A method for preparing nano-emulsion with milk phospholipid as emulsifier according to any one of claims 1-4, which mainly comprises the following steps:
s1: heating water to 50-80 deg.C, adding milk phospholipid, and mixing to obtain hydrated milk phospholipid emulsifier;
s2: uniformly mixing the functional grease and the hydrated milk phospholipid emulsifier prepared in the step S1, and homogenizing for at least 1 time in a homogenizer with the pressure of 20-40Mpa to obtain a crude emulsion;
s3: and (3) putting the coarse emulsion prepared in the step (S2) in a high-pressure homogenizer with the pressure of 100-150Mpa for at least 1 time to obtain the nano emulsion taking the milk phospholipid as the emulsifier.
6. The method for preparing nano-emulsion by using milk phospholipid as emulsifier according to claim 5, wherein in the step S1, the mixing mode is mechanical stirring, the rotating speed is 800-1000r/min, and the stirring time is 10-120min.
7. The method of claim 5, wherein the number of homogenization steps is 1-3, in step S3.
8. Use of a nanoemulsion of any of claims 1 to 4 with milk phospholipids as emulsifier in food products.
CN202210934416.5A 2022-08-04 2022-08-04 Nano emulsion taking milk phospholipid as emulsifier and preparation method and application thereof Pending CN115251363A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114832001A (en) * 2022-05-12 2022-08-02 北京素维生物科技有限公司 Phospholipid composition without auxiliary emulsifier and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106723052A (en) * 2016-12-28 2017-05-31 广东澳米嘉生物科技有限公司 A kind of preparation method of the linseed oil nanoemulsions rich in ω 3
CN113826906A (en) * 2021-11-16 2021-12-24 蕴能(大连)生物科技有限公司 Dihydroquercetin nanoemulsion and preparation method and application thereof
CN114680180A (en) * 2020-12-29 2022-07-01 丰益(上海)生物技术研发中心有限公司 A concentrated emulsion containing low concentration plant phospholipid with high lipid digestibility

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106723052A (en) * 2016-12-28 2017-05-31 广东澳米嘉生物科技有限公司 A kind of preparation method of the linseed oil nanoemulsions rich in ω 3
CN114680180A (en) * 2020-12-29 2022-07-01 丰益(上海)生物技术研发中心有限公司 A concentrated emulsion containing low concentration plant phospholipid with high lipid digestibility
CN113826906A (en) * 2021-11-16 2021-12-24 蕴能(大连)生物科技有限公司 Dihydroquercetin nanoemulsion and preparation method and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114832001A (en) * 2022-05-12 2022-08-02 北京素维生物科技有限公司 Phospholipid composition without auxiliary emulsifier and preparation method thereof

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