Preparation method of easy-to-oxidize functional lipid self-emulsifying emulsion

Abstract

The invention discloses a preparation method of an easy-to-oxidize functional lipid self-emulsifying emulsion, which comprises the following steps: step 1, uniformly dissolving glycerol and sugar alcohol in water at 1-4 DEG C to obtain a water phase part; 2, placing phospholipid in a vacuum environment at 60-110 DEG C, and stirring to enable the phospholipid to be completely liquefied to serve as an emulsifier part; 3, placing the functional lipid in an environment of 1-4 DEG C as an oil phase part; and 4, feeding the water phase part in the step 1, the emulsifier part in the step 2 and the oil phase part in the step 3 through three pipelines respectively, feeding 15-72% of the water phase part, 3-20% of the emulsifier part and 25-65% of the oil phase part into an emulsification pump, instantaneously feeding the oil phase part at low temperature, and carrying out high-speed shearing and homogenizing treatment to form the self-emulsifying emulsion. The bioavailability and oxidation stability of the functional lipid can be improved, meanwhile, the potential health problem caused by synthesis of a surfactant in the prior art is solved, and a solution is provided for efficient delivery of different types of functional lipid.

Description

Technical Field

[0001] The invention relates to the field of food processing, and in particular to a method for preparing an easily oxidizable functional lipid self-emulsifying emulsion. Background Art

[0002] Fish oil, a natural product rich in ω-3 polyunsaturated fatty acids (such as EPA and DHA), is widely used in the fields of functional foods, medicines and nutritional supplements due to its significant effects in regulating blood lipids, anti-inflammation, neuroprotection and promoting cardiovascular health. In recent years, as people's attention to health continues to increase, the market demand for fish oil products has continued to grow. Although fish oil has many health benefits, its strong hydrophobicity leads to extremely low solubility in water, which in turn limits its absorption efficiency in the body. In addition, the highly unsaturated double bond structure in fish oil molecules makes it prone to oxidative degradation and hydrolytic rancidity during processing, storage and transportation, which not only affects the quality and stability of the product, but also may produce harmful oxidation products, bringing potential safety issues. Therefore, how to improve the bioavailability and stability of fish oil is a key issue that needs to be urgently addressed in the current fields of food science and nutrient delivery technology.

[0003] In recent years, self-emulsifying formulations have garnered widespread attention due to their potential to significantly improve the bioavailability of water-insoluble ingredients. Self-emulsifying formulations, through the synergistic action of surfactants and an oil phase, spontaneously form nano- or micron-sized emulsion droplets under mild conditions. This significantly increases the specific surface area of lipids, thereby promoting the efficient contact between lipids and digestive enzymes and enhancing their absorption in the body. However, traditional self-emulsifying formulations rely on synthetic surfactants such as polysorbates. Despite their excellent emulsifying properties, long-term ingestion can cause intestinal barrier dysfunction, limiting their potential for application in functional foods. Phospholipids, as naturally amphiphilic molecules, combine emulsification and biocompatibility, making them an ideal candidate for constructing green self-emulsifying systems. The hydrophilic head and hydrophobic tail of phospholipids impart unique interfacial activity, promoting emulsion formation by reducing oil-water interfacial tension and stabilizing the droplet structure through hydrophobic interactions. Studies have shown that phospholipids can effectively reduce oil-water interfacial tension, promote emulsion formation, and stabilize the droplet structure through hydrophobic interactions, thereby improving emulsion stability. However, the self-emulsifying properties of phospholipids are significantly affected by their molecular structure, concentration and synergistic effects with other components.

[0004] Although there have been studies on the use of phospholipids to construct self-emulsifying systems, there is still a lack of systematic research in the prior art on the effects of natural phospholipids in the self-emulsification process of fish oil and their regulation of the absorption capacity of fish oil in the body. In addition, the prior art has not conducted in-depth discussions on the differences in self-emulsification effects and bioavailability improvements of different fish oil types (such as ethyl ester type and triglyceride type). Therefore, it is of great scientific significance and application value to develop an efficient, stable and biocompatible fish oil delivery system to improve the bioavailability and stability of fish oil, while solving the potential health problems caused by synthetic surfactants in the prior art and providing solutions for the efficient delivery of different types of lipids. Summary of the Invention

[0005] In order to solve the technical problems existing in the prior art, the purpose of this application is to provide a method for preparing an easily oxidizable functional lipid self-emulsifying emulsion, which can improve the bioavailability and oxidative stability of functional lipids, while solving the potential health problems caused by synthetic surfactants in the prior art and providing solutions for the efficient delivery of different types of lipids.

[0006] In order to solve the above-mentioned existing technical problems, the purpose of this application is achieved by adopting the following technical solution: a method for preparing an easily oxidizable functional lipid self-emulsifying emulsion, comprising the following steps:

[0007] Step 1: Dissolve glycerol and sugar alcohol evenly in water at 1-4°C as the aqueous phase;

[0008] Step 2: Place the phospholipid in a vacuum environment at 60-110°C and stir to completely liquefy it, which serves as the emulsifier;

[0009] Step 3: Place the functional lipids in an environment of 1-4°C as the oil phase;

[0010] Step 4: The water phase part in step 1, the emulsifier part in step 2, and the oil phase part in step 3 are fed into three pipelines respectively, and are fed into the emulsification pump according to 15-72% water phase part, 3-20% emulsifier part, and 25-65% oil phase part. The oil phase part is fed instantaneously at low temperature and subjected to high-speed shear homogenization treatment to form a self-emulsifying emulsion.

[0011] Preferably, in the step 1, the concentration of glycerol and sugar alcohol dissolved in the aqueous phase is 1-12 wt %; and the weight ratio of glycerol to sugar alcohol is 1:9 to 5:2.

[0012] Preferably, the sugar alcohol includes one or more of maltitol, sorbitol, xylitol, erythritol, isomalt, lactitol, and mannitol.

[0013] Preferably, the stirring time in step 2 is 30-90 min; the complete liquefaction characteristic is that the dynamic viscosity is less than 500 Pa·s and the liquid is in a transparent and uniform state.

[0014] Preferably, the phospholipids include one or more of lecithin, soybean lecithin, glyceryl monostearate, sucrose fatty acid esters, Tween series, Span series, and polyglycerol fatty acid esters.

[0015] Preferably, the functional lipids include one or more of fish oil, krill oil, astaxanthin oil, algae oil, vitamin oil, conjugated linoleic acid, phytosterols, phytostanols, phosphatidylserine, coconut oil, palm oil, corn oil, soybean oil, evening primrose oil, pumpkin seed oil, sunflower seed oil, linseed oil, sesame oil, sea buckthorn oil, walnut oil, safflower seed oil, perilla seed oil, wheat germ oil, camellia seed oil, ganoderma lucidum spore oil, Xanthoceras sorbifolia oil, Acer truncatum seed oil, and peony seed oil.

[0016] Preferably, the fish oil is in the ethyl ester type or the triglyceride type.

[0017] Preferably, the ratio of EPA to DHA in the fish oil is 5-18:12-25.

[0018] Preferably, the feed temperature of the oil phase in step 4 is instantaneously reduced to -40 to -20°C.

[0019] Preferably, the feed temperature of the oil phase in step 4 is instantaneously reduced to -25°C.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] The method for preparing a self-emulsifying emulsion of easily oxidizable functional lipids using the above technical solution can improve the bioavailability and oxidative stability of functional lipids, while solving the potential health problems caused by synthetic surfactants in the existing technology and providing solutions for the efficient delivery of different types of lipids. DETAILED DESCRIPTION

[0022] Below, the present application is further described in conjunction with specific implementation methods. It should be noted that, under the premise of no conflict, the various embodiments or technical features described below can be arbitrarily combined to form new embodiments.

[0023] In the description of this application, it should be understood that the terms "up", "down", "left", "right", etc. indicate directions or positional relationships, which are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and therefore cannot be understood as a limitation on this application.

[0024] A method for preparing an easily oxidizable functional lipid self-emulsifying emulsion comprises the following steps:

[0025] Step 1: Evenly dissolving glycerol and sugar alcohol in water at 1-4°C as the aqueous phase, wherein the concentration of glycerol and sugar alcohol dissolved in the aqueous phase is 1-12 wt%; and the weight ratio of glycerol to sugar alcohol is 1:9 to 5:2;

[0026] Step 2: Place the phospholipid in a vacuum environment at 60-110°C and stir until it is completely liquefied. As the emulsifier, the stirring time is 30-90 minutes. The characteristics of complete liquefaction are dynamic viscosity less than 500 Pa·s and a transparent and uniform state.

[0027] Step 3: Place the functional lipids in an environment of 1-4°C as the oil phase;

[0028] Step 4: The water phase part in step 1, the emulsifier part in step 2, and the oil phase part in step 3 are fed into three pipelines respectively, and are fed into the emulsification pump according to 15-72% water phase part, 3-20% emulsifier part, and 25-65% oil phase part. The oil phase part is instantaneously cooled to -40 to -20°C and fed, and high-speed shear homogenization treatment is performed to form a self-emulsifying emulsion.

[0029] The sugar alcohol includes one or more of maltitol, sorbitol, xylitol, erythritol, isomalt, lactitol, and mannitol.

[0030] The phospholipids include one or more of lecithin, soybean lecithin, glyceryl monostearate, sucrose fatty acid esters, Tween series, Span series, and polyglycerol fatty acid esters.

[0031] The functional lipids include one or more of fish oil, krill oil, astaxanthin oil, algae oil, vitamin oil, conjugated linoleic acid, phytosterols, phytostanols, phosphatidylserine, coconut oil, palm oil, corn oil, soybean oil, evening primrose oil, pumpkin seed oil, sunflower seed oil, linseed oil, sesame oil, sea buckthorn oil, walnut oil, safflower seed oil, perilla seed oil, wheat germ oil, camellia seed oil, ganoderma lucidum spore oil, Xanthoceras sorbifolia oil, Acer truncatum seed oil, and peony seed oil.

[0032] The fish oil is of ethyl ester type or triglyceride type, and the ratio of EPA to DHA in the fish oil is 5-18:12-25.

[0033] The above-mentioned method for preparing a self-emulsifying emulsion of easily oxidizable functional lipids can improve the bioavailability and oxidative stability of functional lipids, while solving the potential health problems caused by synthetic surfactants in the existing technology and providing solutions for the efficient delivery of different types of lipids.

[0034] The technical effects of the present invention are described below with reference to comparisons of several experimental examples.

[0035] Experimental Examples 1 and 2 adopt dual-channel feeding.

[0036] Experimental Example 1:

[0037] A 6% (w / w) dose of phospholipid and ethyl ester fish oil was placed in a vacuum environment at 85°C and stirred for 60 minutes to completely liquefy it (dynamic viscosity <500 Pa·s, transparent and uniform state); then dispersed at 12000 rpm for 5 minutes; then circulated through a 120 MPa high-pressure microfluidizer for three times to prepare an emulsion; and using dual-channel feeding, mixed with water containing 3wt% glycerol and sugar alcohol, and homogenized at 5000 rpm for 30 seconds to obtain a fish oil phospholipid self-emulsifying emulsion.

[0038] The obtained fish oil lecithin self-emulsifying emulsion has poor oxidative stability and its peroxide value increases after short-term standing.

[0039] Experimental Example 2:

[0040] A 6% (w / w) dose of phospholipid and ethyl ester fish oil was placed in a vacuum environment at 25°C and stirred for 60 minutes to completely liquefy it (dynamic viscosity <500 Pa·s, transparent and uniform state); then dispersed at 12000 rpm for 5 minutes; then circulated through a 120 MPa high-pressure microfluidizer for three times to prepare an emulsion; and using dual-channel feeding, mixed with water containing 3wt% glycerol and sugar alcohol, and homogenized at 5000 rpm for 30 seconds to obtain a fish oil phospholipid self-emulsifying emulsion.

[0041] Compared with Experimental Example 1, the temperature of the vacuum environment is lowered, and the dynamic viscosity of the emulsion prepared in the middle is extremely large, making it difficult to disperse into oil droplets and be wrapped by the water phase during the homogenization process; the fish oil lecithin self-emulsifying emulsion finally prepared contains a large amount of unemulsified oil phase with a large area and irregular shape.

[0042] Experimental Example 3 adopts three-channel feeding and uses pure water as the aqueous phase.

[0043] Experimental Example 3:

[0044] A three-channel feeding emulsification method was used. The phospholipid was placed in a vacuum environment at 85°C and stirred for 60 minutes to completely liquefy it (dynamic viscosity <500 Pa·s, transparent and uniform state) and then introduced into the emulsifier channel. Ethyl ester fish oil was placed in an environment at 4°C and introduced into the oil phase channel. Pure water was introduced into the water phase channel. The three-channel mixture was subjected to high-speed shear homogenization treatment at 5000 rpm for 30 seconds to obtain a fish oil phospholipid self-emulsifying emulsion.

[0045] Compared with Experimental Example 1, the prepared fish oil phospholipid emulsion was very viscous, had a large apparent dynamic viscosity, and had an uneven distribution of oil droplet sizes. After being prepared into fish oil soft capsules, some of them burst.

[0046] Experimental Examples 4 to 6 adopted three-channel feeding, and water dissolved with glycerol and sugar alcohol was used as the aqueous phase.

[0047] Experimental Example 4:

[0048] A three-channel feeding emulsification method was used. The phospholipid was placed in a vacuum environment at 85°C and stirred for 60 minutes to completely liquefy it (dynamic viscosity <500 Pa·s, transparent and uniform state) and then introduced into the emulsifier channel. Ethyl ester fish oil was placed in an environment at 4°C and introduced into the oil phase channel. Water containing 3wt% glycerol and sugar alcohol was introduced into the aqueous phase channel. The three-channel mixture was subjected to high-speed shear homogenization treatment at 5000 rpm for 30 seconds to obtain a fish oil phospholipid self-emulsifying emulsion.

[0049] Compared with Experimental Example 3, it can be seen that the self-emulsifying emulsion of fish oil lecithin with the addition of glycerol and sugar alcohol is stable, has improved fluidity, reduced apparent dynamic viscosity, smaller oil droplet size and uniform distribution, and the prepared fish oil soft capsules are stable and do not break when left standing.

[0050] Experimental Example 5:

[0051] A three-channel feeding emulsification method was used. The phospholipid was placed in a vacuum environment at 85°C and stirred for 60 minutes to completely liquefy it (dynamic viscosity <500 Pa·s, transparent and uniform state) and then introduced into the emulsifier channel. Ethyl ester fish oil was placed in an environment at 4°C and introduced into the oil phase channel. Water containing 6wt% glycerol and sugar alcohol was introduced into the aqueous phase channel. The three-channel mixture was subjected to high-speed shear homogenization treatment at 5000 rpm for 30 seconds to obtain a fish oil-phospholipid self-emulsifying emulsion.

[0052] The stability of the prepared fish oil lecithin self-emulsifying emulsion is further improved, the fluidity is further optimized, the apparent dynamic viscosity is reduced, the oil droplet size is reduced, there is no obvious agglomeration phenomenon, and the texture of the fish oil soft capsule is stable.

[0053] Experimental Example 6:

[0054] A three-channel feeding emulsification method was used. The phospholipid was placed in a vacuum environment at 85°C and stirred for 60 minutes to completely liquefy it (dynamic viscosity <500 Pa·s, transparent and uniform state) and then introduced into the emulsifier channel. Ethyl ester fish oil was placed in an environment at 4°C and introduced into the oil phase channel. Water containing 10wt% glycerol and sugar alcohol was introduced into the aqueous phase channel. The three-channel mixture was subjected to high-speed shear homogenization treatment at 5000 rpm for 30 seconds to obtain a fish oil-phospholipid self-emulsifying emulsion.

[0055] The stability of the prepared fish oil lecithin self-emulsifying emulsion is significantly improved, it can flow smoothly, the apparent dynamic viscosity is greatly reduced, and the oil droplets are evenly dispersed in the aqueous phase at a uniform smaller scale. After being made into fish oil soft capsules, the physical and oxidative stability at room temperature is significantly improved.

[0056] Experimental Example 7 adopts three-channel feeding, and water dissolved with glycerol and sugar alcohol is used as the aqueous phase, and the oil phase is instantaneously fed at low temperature for emulsification.

[0057] Experimental Example 7:

[0058] The oil phase is instantaneously fed at low temperature for emulsification. The phospholipid is placed in a vacuum environment at 85°C and stirred for 60 minutes to completely liquefy it (dynamic viscosity <500 Pa·s, transparent and uniform), and then introduced into an emulsifier channel. Ethyl ester fish oil is placed in a 4°C environment and introduced into the oil phase channel. 4°C water containing 3wt% glycerol and sugar alcohol is introduced into the water phase channel. The oil phase is instantaneously fed at low temperature to -25°C. The three-channel mixture is subjected to high-speed shear homogenization treatment at 5000 rpm for 30 seconds to obtain a fish oil phospholipid self-emulsifying emulsion.

[0059] The fish oil lecithin self-emulsifying emulsion prepared by instantaneous low-temperature feeding emulsification of the oil phase maintains a stable state, improves fluidity, reduces apparent dynamic viscosity, and reduces and evenly distributes the oil droplets. After being made into fish oil soft capsules, they are stable and do not break when left standing. After long-term storage, the flavor is stable and there is no obvious oxidation phenomenon.

[0060] From the comparison of Experimental Example 4, Experimental Example 5, Experimental Example 6, and Example 7, it can be seen that the increase in the content of glycerol and sugar alcohol and the decrease in the temperature of the emulsification process can improve the physical stability and oxidative stability of the fish oil self-emulsifying emulsion, reduce the oil droplet size, and make the distribution more uniform.

[0061] Example 7 is an example of the present application, which can improve the bioavailability and oxidative stability of fish oil, while solving the potential health problems caused by synthetic surfactants in the prior art and providing a solution for the efficient delivery of different types of functional lipids.

[0062] The above-mentioned embodiments are only preferred embodiments of the present application and cannot be used to limit the scope of protection of the present application. Any non-substantial changes and replacements made by technicians in this field based on the present application shall fall within the scope of protection required by the present application.

Claims

1. A method for preparing an easily oxidizable functional lipid self-emulsifying emulsion, characterized in that: The following steps are involved: Step 1: Dissolve glycerol and sugar alcohol evenly in water at 1-4°C as the aqueous phase; Step 2: Place the phospholipid in a vacuum environment at 60-110°C and stir to completely liquefy it, which serves as the emulsifier; Step 3: Place the functional lipids in an environment of 1-4°C as the oil phase; Step 4: The water phase part in step 1, the emulsifier part in step 2, and the oil phase part in step 3 are fed into three pipelines respectively, and are fed into the emulsification pump according to 15-72% water phase part, 3-20% emulsifier part, and 25-65% oil phase part. The oil phase part is fed instantaneously at low temperature and subjected to high-speed shear homogenization treatment to form a self-emulsifying emulsion.

2. The method for preparing a self-emulsifying emulsion of an easily oxidizable functional lipid according to claim 1, wherein: In the step 1, the concentration of glycerol and sugar alcohol dissolved in the aqueous phase is 1-12 wt %; the weight ratio of glycerol to sugar alcohol is 1:9 to 5:

2.

3. The method for preparing a self-emulsifying emulsion of an easily oxidizable functional lipid according to claim 1 or 2, wherein: The sugar alcohol includes one or more of maltitol, sorbitol, xylitol, erythritol, isomalt, lactitol, and mannitol.

4. The method for preparing a self-emulsifying emulsion of easily oxidizable functional lipids according to claim 1, wherein: The stirring time in step 2 is 30-90 minutes; the complete liquefaction characteristic is that the dynamic viscosity is less than 500 Pa·s and the liquid is in a transparent and uniform state.

5. The method for preparing a self-emulsifying emulsion of easily oxidizable functional lipids according to claim 1 or 4, wherein: The phospholipids include one or more of lecithin, soybean lecithin, glyceryl monostearate, sucrose fatty acid esters, Tween series, Span series, and polyglycerol fatty acid esters.

6. The method for preparing a self-emulsifying emulsion of easily oxidizable functional lipids according to claim 1, wherein: The functional lipids include one or more of fish oil, krill oil, astaxanthin oil, algae oil, vitamin oil, conjugated linoleic acid, phytosterols, phytostanols, phosphatidylserine, coconut oil, palm oil, corn oil, soybean oil, evening primrose oil, pumpkin seed oil, sunflower seed oil, linseed oil, sesame oil, sea buckthorn oil, walnut oil, safflower seed oil, perilla seed oil, wheat germ oil, camellia seed oil, ganoderma lucidum spore oil, Xanthoceras sorbifolia oil, Acer truncatum seed oil, and peony seed oil.

7. The method for preparing a self-emulsifying emulsion of easily oxidizable functional lipids according to claim 6, wherein: The fish oil is in ethyl ester type or triglyceride type.

8. The method for preparing a self-emulsifying emulsion of easily oxidizable functional lipids according to claim 7, wherein: The ratio of EPA to DHA in the fish oil is 5-18:12-25.

9. The method for preparing a self-emulsifying emulsion of easily oxidizable functional lipids according to claim 1, wherein: In the step 4, the feed temperature of the oil phase is instantly reduced to -40 to -20°C.

10. The method for preparing a self-emulsifying emulsion of easily oxidizable functional lipids according to claim 9, wherein: In the step 4, the feed temperature of the oil phase is instantly reduced to -25°C.