A high oil load lanolin powder grease and a method of making the same

By using Pickering emulsion technology and plant polyphenol-modified interfaces, the problems of low oil loading and poor rehydration of mutton fat powder have been solved, achieving the preparation of mutton fat powder with high oil loading and healthy properties, which is suitable for food production.

CN119054752BActive Publication Date: 2026-05-15JIANGNAN UNIV
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202411351659.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-26
Publication Date
2026-05-15
Estimated Expiration
2044-09-26

AI Technical Summary

Technical Problem

Existing technologies for sheep fat powder have low oil loading capacity, low yield, low encapsulation rate, poor rehydration properties, and the use of small molecule emulsifiers poses potential harm to the human body.

Method used

Using Pickering emulsion technology, composite particles are constructed using gelatin, nanocellulose, and nonionic cellulose ethers. Combined with plant polyphenols to modify the emulsion interface, high oil-loading lanolin powder is prepared, avoiding the use of small molecule emulsifiers.

Benefits of technology

Sheep fat powder with an oil loading of over 90% was prepared, exhibiting good rehydration properties and health benefits, making it suitable for food production.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119054752B_ABST
    Figure CN119054752B_ABST
Patent Text Reader

Abstract

The application discloses a kind of high oil load mutton oil powder grease and its preparation method, belong to food processing technical field.The method is as follows: (1) preparation gelatin solution, join nanocellulose stirring to obtain composite liquid, then adjust pH, the non-ionic cellulose ether of addition is carried out high pressure homogenization to obtain suspension, then dry to obtain nanocomposite particle;(2) the nanocomposite particle in step (1) is dispersed in water as aqueous phase system, mutton oil is added as oil phase in aqueous phase and is sheared, high pressure homogenization obtains mutton oil pickering emulsion;(3) the mutton oil pickering emulsion of step (2) is added in plant polyphenol, and the modified mutton oil pickering emulsion is obtained;(4) the modified mutton oil pickering emulsion in step (3) is spray dried to obtain mutton oil powder grease.The application makes the oil load of mutton oil powder grease reach 90% without adding any small molecule surfactant, and mutton oil powder grease has good rehydration.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention belongs to the field of food processing technology, specifically relating to a high-oil-loading mutton fat powder and its preparation method. Background Technology

[0002] Powdered oils are uniformly sized powdered products formed by encapsulating oils with appropriate wall materials using microencapsulation technology. They are widely used in solid beverages, baking, soup mixes, ice cream, and functional food industries, and have become an important raw material and carrier for modern food processing and manufacturing. Mutton fat has functions such as improving the taste and flavor of food and providing energy; however, it suffers from problems such as easy oxidation and difficulty in dispersion during food processing and storage, seriously affecting its processing and application. Microencapsulating mutton fat into powdered oils can effectively improve its workability, increase its water solubility and dispersibility, and enhance its storage stability. Therefore, the development of mutton fat powdered oils is of great significance for the development of mutton fat itself and related downstream industries.

[0003] However, the preparation of traditional powdered greases requires the addition of a large amount of wall material, resulting in generally low oil loading capacity. Even with increased oil loading, mutton fat powdered greases are prone to problems such as low yield, low encapsulation efficiency, and poor rehydration. Furthermore, the preparation of traditional powdered greases still requires the use of small-molecule emulsifiers, which pose potential health risks. Therefore, there is a need for a healthy mutton fat powdered grease that does not use small-molecule emulsifiers, has high oil loading capacity, good rehydration properties, and is formulated without the use of small-molecule emulsifiers. Summary of the Invention

[0004] To address the aforementioned problems, this invention provides a high-oil-loading lanolin powder grease based on Pickering emulsion and its preparation method. The prepared lanolin powder grease has an oil loading of up to 90% or more, exhibits excellent rehydration properties in warm water, and requires no added small-molecule emulsifiers.

[0005] This invention provides a high oil-loading mutton fat powder, which is made from the following raw materials by mass fraction: 7-12% composite particles, 85-92% mutton fat, and 1-5% plant polyphenols.

[0006] Preferably, the high oil-loading mutton fat powder is made from the following raw materials by mass fraction: 9-10% composite particles, 87-90% mutton fat, and 1-3% plant polyphenols.

[0007] Furthermore, the composite particles are composed of gelatin, nanocellulose, and nonionic cellulose ether.

[0008] Furthermore, the sources of nanocellulose include commercial purchases or preparation methods.

[0009] Furthermore, the preparation method of nanocellulose is as follows: microcrystalline cellulose is hydrolyzed with 50-70 wt% sulfuric acid at a material-to-liquid ratio of 1 g: 10-20 mL for 30-60 min. After hydrolysis, the precipitate is collected by centrifugation, the precipitate is dispersed in water, and then dialyzed using an 8-14 kDa dialysis bag. Finally, the dialysate is dried to obtain nanocellulose.

[0010] Furthermore, the nonionic cellulose ether is selected from methylcellulose, hydroxypropyl methylcellulose, hydroxyethylcellulose, or hydroxypropylcellulose.

[0011] Furthermore, in the composite particles, the mass ratio of gelatin to nanocellulose is 1:0.5–2; the mass ratio of gelatin to nonionic cellulose ether is 1:0.5–2.

[0012] Preferably, in the composite particles, the mass ratio of gelatin to nanocellulose is 1:1 to 2; the mass ratio of gelatin to nonionic cellulose ether is 1:1 to 2.

[0013] Furthermore, the plant polyphenols are one or more of gallic acid, tannic acid, and catechins.

[0014] Preferably, the plant polyphenol is tannic acid.

[0015] This invention also provides a method for preparing mutton fat powder, the method comprising the following steps:

[0016] (1) Preparation of Pickering emulsion particles: Gelatin was dissolved in water by heating to prepare a gelatin solution. Then, nanocellulose was added and stirred to obtain a composite solution. The pH of the composite solution was then adjusted to 3.0-4.5. Then, nonionic cellulose ether was added and subjected to high pressure homogenization to obtain a suspension. The suspension was then dried to obtain nanocomposite particles.

[0017] (2) Preparation of emulsion: The nanocomposite particles in step (1) are dispersed in water as an aqueous phase system, and mutton fat is added to the aqueous phase as an oil phase for shearing and high-pressure homogenization to obtain mutton fat Pickering emulsion.

[0018] (3) Emulsion modification: Plant polyphenols were added to the lanolin pickering emulsion from step (2), and the mixture was stirred and sonicated to obtain the modified lanolin pickering emulsion.

[0019] (4) Preparation of powdered oil: The modified lanolin emulsion in step (3) is spray-dried to obtain lanolin powdered oil.

[0020] Furthermore, the nanocellulose in step (1) is prepared by the following method: microcrystalline cellulose is hydrolyzed with 50-70wt% sulfuric acid at a material-to-liquid ratio of 1g:10-20mL for 30-60min. After hydrolysis, the precipitate is collected by centrifugation, the precipitate is dispersed in water, and then dialyzed with an 8-14kDa dialysis bag. Finally, the dialysate is dried to obtain nanocellulose.

[0021] Furthermore, the concentration of the gelatin solution in step (1) is 0.5–2 wt%.

[0022] Furthermore, in step (1), the mass ratio of gelatin to nanocellulose is 1:0.5 to 2.

[0023] Furthermore, in step (1), the nonionic cellulose ether is selected from methylcellulose, hydroxypropyl methylcellulose, hydroxyethylcellulose or hydroxypropylcellulose.

[0024] Furthermore, in step (1), the mass ratio of gelatin to nonionic cellulose ether is 1:0.5 to 2.

[0025] Preferably, the mass ratio of gelatin to nanocellulose in step (1) is 1:1 to 2.

[0026] Preferably, the mass ratio of gelatin and nonionic cellulose ether in step (1) is 1:1 to 2.

[0027] Furthermore, in step (2), the concentration of the composite particles in the aqueous phase is 1–5%, g / mL.

[0028] Furthermore, in step (2), the mass ratio of composite particles to oil phase is 1.5 to 2.5:20.

[0029] Furthermore, the shearing parameters in step (2) are 5000-15000 rpm and 1-10 min.

[0030] Furthermore, in step (2), the parameters for high-pressure homogenization are 20-50 MPa, and homogenization is performed 1-5 times.

[0031] Furthermore, in step (3), the plant polyphenols are one or more of gallic acid, tannic acid, and catechin.

[0032] Preferably, the plant polyphenol in step (3) is tannic acid.

[0033] Furthermore, in step (3), the amount of plant polyphenols added is 20-25% of the mass of the composite particles.

[0034] Furthermore, in step (3), the ultrasound parameters are 400–600W and 10–20min.

[0035] Furthermore, the spray drying conditions in step (4) are: inlet temperature 150℃~170℃, outlet temperature 80℃~90℃, and flow rate 0.4~0.6L / h.

[0036] This invention provides mutton fat powder prepared according to the above method.

[0037] The application of the mutton fat powder provided by this invention in the food industry.

[0038] Furthermore, the application refers to its use as a food ingredient in the preparation of hot pot base, seasonings, meat products, baked goods, prepared foods, and soup bases.

[0039] The beneficial effects of this invention are:

[0040] This invention uses nanocellulose as Pickering emulsion particles. Through electrostatic interactions and the affinity between cellulose molecules, easily film-forming gelatin and cellulose ethers are sequentially introduced onto the surface of the nanocellulose to construct a low-solids dry basis lanolin Pickering emulsion. Subsequently, the emulsion interface is further modified and reinforced in situ using the interactions between plant polyphenols, proteins, and cellulose ethers to prevent emulsion demulsification during spray drying. Ultimately, without adding any small-molecule surfactants, the lanolin powder achieves an oil loading of up to 90%, resulting in a healthy lanolin powder with a high oil loading. Furthermore, this lanolin powder exhibits good rehydration properties, making it suitable for application in food production. Attached Figure Description

[0041] Figure 1 It consists of high-oil-loading mutton fat powder and oil, as well as rehydrated emulsions. Detailed Implementation

[0042] The preferred embodiments of the present invention are described below. It should be understood that the embodiments are for better explanation of the present invention and are not intended to limit the present invention.

[0043] Measurement indicators of powdered oils

[0044] Oil loading: Weigh approximately 1g of powdered oil and add it to 10mL of 2mol / L HCl solution. Stir for 30min to rupture the capsule wall. Then add 40mL of chloroform and 10mL of methanol, and stir again for 30min. Next, centrifuge at 10000rpm / min for 10min, collect the organic phase, dry it, and weigh the remaining oil. The calculation formula is as follows:

[0045]

[0046] Surface oil content: Add approximately 1g of powdered oil to 15mL of petroleum ether and stir gently for 1 minute. Then filter the mixture through rapid filter paper and wash the residue again with 10mL of petroleum ether. Combine the filtrates and place them in an oven at 60°C until the solvent is completely evaporated. Then collect the residual oil and weigh it, calculating the amount using the following formula:

[0047]

[0048] Encapsulation efficiency: The encapsulation efficiency of the powder is calculated based on the oil loading and surface oil content of the powder. The calculation formula is as follows:

[0049]

[0050] Solubility: Disperse 0.5g of powdered oil in 50℃ warm water, stir magnetically for 20min, then filter. Collect the filter residue, heat to constant weight at 105℃, and weigh. The calculation formula is as follows:

[0051]

[0052] Source of raw materials

[0053] Preparation of nanocellulose: 80g of microcrystalline cellulose was slowly added to 60% sulfuric acid at a material-to-liquid ratio of 1:15 (g / mL) for hydrolysis for 40 min. After the reaction was completed, the reaction was immediately terminated with 10 times the volume of deionized water. The supernatant was then removed by centrifugation, and the precipitate was collected. The precipitate was redispersed in deionized water and dialyzed using an 8-14 kDa dialysis bag to remove excess inorganic salt ions. The precipitate was then dried to obtain nanocellulose. Unless otherwise specified, all raw materials used in the examples were commercially available.

[0054] Example 1

[0055] (1) Disperse gelatin in deionized water and heat to dissolve it to prepare a 1wt% gelatin solution. Then, add nanocellulose crystals to the gelatin solution at a weight ratio of 1:1 (w / w) to gelatin and stir thoroughly to obtain a gelatin-nanocellulose composite solution. Next, adjust the pH of the composite solution to 4.0 and stir continuously so that the negatively charged nanocellulose crystals and the positively charged gelatin attract each other to form composite particles. Then, add methylcellulose at a weight ratio of 1:1 (w / w) to gelatin and further homogenize the composite system under high pressure (30MPa, homogenize twice) to obtain a uniform cellulose ether-nanocellulose-gelatin composite particle suspension. After drying, obtain nanocomposite particles.

[0056] (2) Preparation of emulsion: 2.1g of composite particles (containing 0.7g gelatin, 0.7g nanocellulose crystals, and 0.7g methylcellulose) were dispersed in 80g of deionized water as the aqueous phase system, and mutton fat was melted at 60℃ as the oil phase of the emulsion. First, the aqueous phase system of the nanocellulose-gelatin composite particle suspension was preheated at 60℃ for 5min. Then, 20g of melted mutton fat was added to the aqueous phase system. The mixture was then treated at a shear rate of 10000rpm for 3min to obtain a crude emulsion. Finally, the crude emulsion was subjected to high-pressure homogenization at a pressure of 40MPa, and homogenized twice to obtain a mutton fat Pickering emulsion.

[0057] (3) Emulsion modification: Add 0.5g gallic acid to the lanolin pickering emulsion from step (2), stir continuously at 300rpm, and then perform ultrasonic treatment at 600W for 10min to obtain the modified lanolin pickering emulsion.

[0058] (4) Preparation of powdered grease: The emulsion in step (3) is spray-dried to obtain high oil-carrying powdered grease. The spray drying conditions are: inlet temperature 160℃, outlet temperature 80℃, and flow rate 0.6L / h.

[0059] Comparative Example 1

[0060] Unlike Example 1, gelatin is not used in step (1), but the other steps are the same.

[0061] Comparative Example 2

[0062] Unlike Example 1, methylcellulose is not used in step (1), but the rest of the steps are the same.

[0063] Comparative Example 3

[0064] Unlike Example 1, the emulsion modification in step (3) is not performed, but the remaining steps are the same.

[0065] Example 2

[0066] Similar to Example 1, the amount of composite particles added was the same, that is, 2.1g of composite particles were added to 80g of deionized water, and then 20g of mutton fat was added to prepare an emulsion. The difference from Example 1 was that the ratio of composite particles (gelatin: nanocellulose: methylcellulose) in step (1) was different, namely 1:2:1 (containing 0.525g gelatin, 1.05g nanocellulose crystals, and 0.525g methylcellulose), 1:2:2 (containing 0.42g gelatin, 0.84g nanocellulose crystals, and 0.84g methylcellulose), 1:0.5:0.5 (containing 1.05g gelatin, 0.525g nanocellulose crystals, and 0.525g methylcellulose), and 1:0.5:1 (containing 0.84g gelatin, 0.42g nanocellulose crystals, and 0.84g methylcellulose).

[0067] Table 1. Indicators of powdered oils with different composite particle ratios

[0068]

[0069] Table 1 shows that Comparative Examples 1 and 2 had poor encapsulation effects, with low surface oil content and encapsulation rate in the powdered oil. Comparative Example 3 even failed to produce an effective powdered oil, indicating that polyphenol modification is crucial for the preparation of powdered oils with high oil loading. Among the samples with different composite particle ratios, the gelatin:nanocellulose:methylcellulose ratio of 1:2:2 showed the best effect. When the proportion of nanocellulose in the composite particles was low (0.5%), the various indicators of the powdered oil deteriorated.

[0070] Example 3

[0071] Unlike Example 1, the cellulose ether in step (1) was replaced with equal amounts of hydroxypropyl methylcellulose, hydroxyethylcellulose, and hydroxypropylcellulose, while the other steps remained the same.

[0072] Table 2. Indicators of powdered oils with different cellulose ethers

[0073]

[0074]

[0075] As shown in Table 2, the type of cellulose ether has little effect. The oil loading of all samples is greater than 85%, and the solubility of the samples is also as high as 90%.

[0076] Example 4

[0077] Unlike Example 1, the plant polyphenols in step (3) are replaced with equal amounts of tannic acid, catechin, chlorogenic acid and caffeic acid, while the rest of the steps are the same.

[0078] Table 3. Powder oil indexes under different polyphenol treatments

[0079] Group Oil load (%) Surface oil (%) Encapsulation efficiency (%) Solubility (%) gallic acid 87.38±0.94 7.42±1.11 91.51±1.56 90.42±1.77 Tannic acid 92.52±1.84 4.48±1.32 95.15±1.12 95.53±1.36 Catechins 90.42±1.11 12.04±0.93 86.68±1.44 90.11±2.52 chlorogenic acid 84.27±1.45 13.33±0.83 84.18±1.72 88.55±1.21 caffeic acid 80.21±1.29 14.56±0.67 81.84±1.64 85.265±1.62

[0080] Table 3 shows that tannic acid-modified powdered oils showed the best effect, while chlorogenic acid and caffeic acid showed poorer effects. This is because tannic acid has a stronger interaction with gelatin and cellulose ethers, which can better strengthen the emulsion interface and play a protective role.

[0081] The embodiments provided above are not intended to limit the scope of the invention, nor are the described steps intended to limit the order of execution. Any obvious modifications made to the invention by those skilled in the art based on existing common knowledge also fall within the scope of protection defined by the claims.

Claims

1. A high-oil-loading mutton fat powder, characterized in that, The high oil-loading mutton fat powder is made from the following raw materials by mass fraction: 7-12% composite particles, 85-92% mutton fat, and 1-5% plant polyphenols. The composite particles are composed of gelatin, nanocellulose and nonionic cellulose ether in a mass ratio of 1:0.5~2:0.5~2; The nonionic cellulose ether is selected from methylcellulose, hydroxypropyl methylcellulose, hydroxyethylcellulose, or hydroxypropylcellulose; The plant polyphenols are one or more of gallic acid, tannic acid, and catechins; The method for preparing high-oil-loading mutton fat powder is characterized by comprising the following steps: (1) Preparation of Pickering emulsion particles: Gelatin was dissolved in water by heating to prepare a gelatin solution. Then, nanocellulose was added and stirred to obtain a composite solution. The pH of the composite solution was then adjusted to 3.0~4.

5. Then, non-ionic cellulose ether was added and subjected to high pressure homogenization to obtain a suspension. The suspension was then dried to obtain nanocomposite particles. (2) Preparation of emulsion: The nanocomposite particles in step (1) are dispersed in water as an aqueous phase system, and mutton fat is added to the aqueous phase as an oil phase for shearing and high-pressure homogenization to obtain mutton fat Pickering emulsion. (3) Emulsion modification: Plant polyphenols were added to the lanolin pickering emulsion from step (2), and the mixture was stirred and sonicated to obtain the modified lanolin pickering emulsion. (4) Preparation of powdered oil: The modified lanolin emulsion in step (3) is spray-dried to obtain lanolin powdered oil.

2. The high oil-loading mutton fat powder grease according to claim 1, characterized in that, The composite particles are composed of gelatin, nanocellulose and nonionic cellulose ether in a mass ratio of 1:1~2:1~2.

3. The high oil-loading mutton fat powder grease according to claim 1, characterized in that, The plant polyphenols mentioned are tannic acid.

4. The high oil-loading mutton fat powder grease according to claim 1, characterized in that, In step (1), the concentration of the gelatin solution is 0.5~2wt%; the mass ratio of gelatin to nanocellulose is 1:0.5~2; and the mass ratio of gelatin to nonionic cellulose ether is 1:0.5~2.

5. The high oil-loading mutton fat powder grease according to claim 1, characterized in that, In step (2), the concentration of composite particles in the aqueous phase is 1~5%, g / mL; the mass ratio of composite particles to oil phase is 1.5~2.5:

20.

6. The high oil-loading mutton fat powder grease according to claim 1, characterized in that, In step (3), the amount of plant polyphenols added is 20-25% of the mass of the composite particles.

7. The high oil-loading mutton fat powder grease according to claim 1, characterized in that, In step (4), the spray drying conditions are: inlet temperature 150℃~170℃, outlet temperature 80℃~90℃, and flow rate 0.4~0.6 L / h.

8. The application of the high oil-loading mutton fat powder according to any one of claims 1 to 7 in the food industry.

9. The application according to claim 8, characterized in that, The mutton fat powder is used as a food ingredient in the preparation of seasonings, meat products, baked goods, and prepared foods.