Preparation method of fucoxanthin nano-emulsion

Abstract

The invention provides a fucoxanthin nano-emulsion preparation method, and relates to the technical field of biological medicine, fucoxanthin and medium chain triglyceride are used as raw materials to support an oil phase solvent, and the oil phase solvent is mixed with resistant dextrin, isomaltooligosacharide and fructo-oligosaccharide to prepare the fucoxanthin nano-emulsion. The oil-in-water fucoxanthin nano-emulsion with the particle size of 1-100nm is obtained by mixing water-phase solvents prepared from fucoxanthin, blood orange powder and the like, processing by a colloid mill and emulsifying and shearing by a vacuum tank, and the preparation increases the solubility of fucoxanthin, removes the unpleasant odor of fucoxanthin, reduces degradation of gastrointestinal tracts, improves the bioavailability, reduces the toxic and side effects of the fucoxanthin, improves the bioavailability of the fucoxanthin, and improves the bioavailability of the fucoxanthin. The controlled release and absorption of fucoxanthin are realized, and compared with traditional tablets and capsule products, the compliance of females, middle-aged people and old people who have difficulty in swallowing is greatly improved.

Description

Technical Field

[0001] The invention relates to the technical field of biomedicine, and in particular to a method for preparing a fucoxanthin nanoemulsion. Background Art

[0002] Fucoxanthin, also known as fucoxanthin and brown phycoxanthin, is a highly active natural carotenoid that is safe and non-toxic to the human body. Fucoxanthin is like a precise key that can unlock the lock of heat production and lipolysis conversion in fat cells (β3-AR and UPC1), start the combustion engine of fat cell mitochondria, burn fat to generate heat without the need for deliberate exercise and dieting, and achieve static lipid reduction and weight loss. Fucoxanthin has the effect of inhibiting fat production, accelerating the burning of brown fat cells, and promoting the transformation and burning of white fat cells into brown fat cells, thereby reducing the white fat tissue in the abdomen, and fat reduction does not rebound; at the same time, it stimulates the liver to produce DHA, a precious core ingredient that lowers cholesterol levels and brain neurotrophy.

[0003] The prior art has the following technical problems when using weight loss products:

[0004] Non-fucoxanthin weight loss products such as diets and fast food meal replacements are prone to rebound and decreased immunity. Existing fucoxanthin products are in the form of tablets or capsules, which have a strong fishy smell, poor taste, and are easily oxidized. The sealing strength of the hard capsules is not strong enough, and air can easily penetrate into the product, causing the active ingredients to be oxidized during the shelf life and poor stability. Summary of the invention

[0005] Technical issues solved

[0006] In view of the shortcomings of the prior art, the present invention provides a method for preparing a fucoxanthin nanoemulsion, which solves the following problems: weight loss products are prone to health risks and the existing fucoxanthin capsules and tablets are not stable and have poor taste.

[0007] Technical Solution

[0008] To achieve the above objectives, the present invention is implemented by the following technical solutions: A method for preparing a fucoxanthin nanoemulsion, including the preparation method as follows:

[0009] Sp1: Preparation of aqueous phase: Take resistant dextrin, isomaltooligosaccharide, fructooligosaccharide, blood orange powder, L-arabinose, esterified vitamin C, citric acid, kelp polysaccharide, mono- and di-glycerol fatty acid esters, sodium octenyl succinate starch raw materials, add water to the raw materials, heat, stir, dissolve and disperse to obtain a premix liquid aqueous phase;

[0010] Sp2: Preparation of oil phase: Take the fucoxanthin medium-chain triglyceride raw material, stir and dissolve it to obtain a premix liquid oil phase;

[0011] Sp3: Preparation of ultrafine suspension emulsion, the water phase and oil phase prepared by Sp1 and Sp2 are added in proportion and processed by colloid mill twice to obtain ultrafine suspension emulsion;

[0012] Sp4: Preparation of fucoxanthin nanoemulsion. The ultrafine suspension emulsion in Sp3 is added into a vacuum emulsification shearing tank, and after vacuum stirring, emulsification shearing, degassing and canning, the fucoxanthin nanoemulsion is obtained.

[0013] Preferably, the mass percentages of the raw materials of each component in the preparation of the aqueous phase are 5%-15% resistant dextrin, 10%-30% isomaltooligosaccharide, 10%-30% fructooligosaccharide, 1%-5% blood orange powder, 5%-10% L-arabinose, 0.5%-1.0% esterified vitamin C, 0.05%-0.2% citric acid, 1%-2% laminarin, 0.05-0.5% mono- and di-glycerol fatty acid esters, 0.05%-0.5% sodium starch glycolate octenylsuccinate, and 15%-25% purified water raw material.

[0014] Preferably, the heating temperature during the preparation of the water phase is 65° C.-85° C., and the stirring, dissolving and dispersing time is 15 min-30 min.

[0015] Preferably, the mass percentages of the raw materials of each component in the preparation of the oil phase are 0.2%-2% fucoxanthin, 10%-40% medium-chain triglycerides, the temperature environment during stirring is room temperature ≤37°C, and the stirring and mixing time is 5min-10min.

[0016] Preferably, in the preparation of the ultrafine suspension emulsion, the ratio of the water phase to the oil phase is 3:2-9:1, the rotation speed of the colloid mill is 3000-5000 r / min, and the number of colloid mill cycles is 1-3 times.

[0017] Preferably, the shear rate of vacuum emulsification in the preparation of the fucoxanthin nanoparticles is 6000 r / min-11000 r / min, and the shear time of vacuum emulsification is 15 min-30 min.

[0018] Preferably, in the preparation of the fucoxanthin nanoparticles, the degassing vacuum degree of the vacuum emulsification is 0.09-0.1 MPa, the canning temperature is 37° C.-46° C., and the size of the nanoemulsifier is 1-100 nm.

[0019] Beneficial Effects

[0020] The present invention provides a method for preparing a fucoxanthin nanoemulsion. It has the following beneficial effects:

[0021] The present invention adopts fucoxanthin and medium-chain triglyceride as raw materials to support the oil phase solvent, and mixes with the water phase solvent prepared from resistant dextrin, isomaltooligosaccharide, oligofructose, blood orange powder, etc., and then obtains the water-in-oil fucoxanthin nanoemulsion with particles of 1-100nm after colloid mill treatment and political emulsification. The preparation increases the solubility of fucoxanthin, removes the bad smell of fucoxanthin, reduces gastrointestinal degradation, improves bioavailability, and realizes the controlled release and absorption of fucoxanthin. Compared with traditional tablets, the compliance of capsule products for women with dysphagia and middle-aged and elderly people to take the products is greatly improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a preparation method diagram of the present invention;

[0023] Figure 2 This is the in vitro dissolution test diagram of the product at pH 6.8. DETAILED DESCRIPTION

[0024] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Specific embodiment one:

[0026] like Figure 1 As shown, a method for preparing a fucoxanthin nanoemulsion is shown below:

[0027] Sp1: Preparation of aqueous phase: Take resistant dextrin, isomaltooligosaccharide, fructooligosaccharide, blood orange powder, L-arabinose, esterified vitamin C, citric acid, kelp polysaccharide, mono- and di-glycerol fatty acid esters, sodium octenyl succinate starch raw materials, add water to the raw materials, heat, stir, dissolve and disperse to obtain a premix liquid aqueous phase;

[0028] Sp2: Preparation of oil phase: Take the fucoxanthin medium-chain triglyceride raw material, stir and dissolve it to obtain a premix liquid oil phase;

[0029] Sp3: Preparation of ultrafine suspension emulsion, the water phase and oil phase prepared by Sp1 and Sp2 are added in proportion and processed by colloid mill twice to obtain ultrafine suspension emulsion;

[0030] Sp4: Preparation of fucoxanthin nanoemulsion. The ultrafine suspension emulsion in Sp3 is added into a vacuum emulsification shearing tank, and after vacuum stirring, emulsification shearing, degassing and canning, the fucoxanthin nanoemulsion is obtained.

[0031] The mass percentages of the raw materials of each component in the preparation of the aqueous phase are 5%-15% resistant dextrin, 10%-30% isomaltooligosaccharide, 10%-30% fructooligosaccharide, 1%-5% blood orange powder, 5%-10% L-arabinose, 0.5%-1.0% esterified vitamin C, 0.05%-0.2% citric acid, 1%-2% kelp polysaccharide, 0.05-0.5% mono- and diglycerol fatty acid esters, 0.05%-0.5% sodium octenyl succinate starch, and 15%-25% purified water raw material. The heating temperature in the preparation process of the aqueous phase is 65° C.-85° C., and the stirring, dissolving and dispersing time is 15 min-30 min.

[0032] The mass percentages of the raw materials of each component in the preparation of the oil phase are 0.2%-2% fucoxanthin and 10%-40% medium-chain triglycerides, respectively. The temperature environment during stirring is room temperature ≤37° C., and the stirring and mixing time is 5min-10min.

[0033] In the preparation of the ultrafine suspension emulsion, the ratio of the water phase to the oil phase is 3:2-9:1, the rotation speed of the colloid mill is 3000-5000 r / min, and the number of colloid mill cycles is 1-3 times.

[0034] The shear rate of vacuum emulsification in the preparation of fucoxanthin nano-materials is 6000r / min-11000r / min, the shear time of vacuum emulsification is 15min-30min, the degassing vacuum degree of vacuum emulsification in the preparation of fucoxanthin nano-materials is 0.09-0.1MPa, the filling temperature is 37°C-46°C, and the size of nano-emulsifier is 1-100nm.

[0035] Fucoxanthin nanoemulsion can form an oil-in-water (O / W) nanoemulsion with a nanometer size of 1-100nm. The preparation increases the solubility of fucoxanthin, removes the bad smell of fucoxanthin, reduces gastrointestinal degradation, improves bioavailability, realizes controlled release and absorption of fucoxanthin, has excellent taste, uses less additives and auxiliary materials, is easy to carry, and has other excellent characteristics. The microemulsion droplets of fucoxanthin nanoemulsion place fat-soluble fucoxanthin in the core of fat emulsion particles. The outer layer of fucoxanthin is surrounded by hydrophilic molecules. Fucoxanthin can be completely retained in the fat emulsion particles, so that it can maintain a stable state in gastric acid. The particle size of the nano-sized fucoxanthin microemulsion droplets becomes very small, and the specific surface area is significantly increased. After oral administration, the contact area with the intestinal mucosa is significantly increased, which greatly improves the bioavailability of fucoxanthin. The compliance of the liquid nanoemulsion for women with dysphagia and middle-aged and elderly people to take the product has been greatly improved. Specific embodiment 2:

[0037] like Figure 1As shown, according to the preparation method of a fucoxanthin nanoformulation provided in the above specific embodiment 1, an experiment was conducted, wherein the ratio and method are as follows:

[0038] Preparation of aqueous phase: Weigh the following components as raw materials according to mass percentage: 5% resistant dextrin, 30% isomaltooligosaccharide, 10% fructooligosaccharide, 1.8% blood orange powder, 13% L-arabinose, 1.0% esterified vitamin C, 0.2% citric acid, 2% kelp polysaccharide, 0.5% mono- and diglycerol fatty acid esters, 0.5% sodium starch octenylsuccinate, and 25% purified water; add the above raw materials into a vacuum stirring tank, heat, stir, dissolve and disperse to obtain a premix liquid aqueous phase.

[0039] The heating temperature of the water phase is: 85°C

[0040] The stirring, dissolving and dispersing time of the aqueous phase is: 30 min

[0041] Preparation of oil phase: Weigh the following raw materials according to mass percentage: 2% fucoxanthin (algae alcohol-extracted oil), 10% medium-chain triglycerides; add the above raw materials into a vacuum stirring tank, stir and disperse at room temperature to obtain a premix liquid oil phase.

[0042] The stirring and mixing temperature of the oil phase is room temperature ≤ 37°C

[0043] The mixing time of the oil phase is: 10 min

[0044] Preparation of superfine suspension emulsion: Add water phase and oil phase in proportion and subject to colloid mill circulation treatment to obtain superfine suspension emulsion.

[0045] The ratio of water phase to oil phase of ultrafine suspension emulsion is: 88:12

[0046] The colloid mill speed of the ultrafine suspension emulsion is 5000 rpm

[0047] The number of colloid mill cycles for ultrafine suspension emulsion is 2 times

[0048] Preparation of nanoemulsion: adding the ultrafine suspension emulsion into a vacuum emulsification shearing tank, and performing vacuum stirring, emulsification shearing, degassing and canning to obtain a fucoxanthin nanoemulsion.

[0049] The shear speed of vacuum emulsification of nanoemulsion is 8000r / min.

[0050] The shear stirring time of vacuum emulsification of nanoemulsion was 30 min.

[0051] The vacuum degree of vacuum emulsification and degassing of nanoemulsion is 0.09 MPa.

[0052] The filling temperature of the nanoemulsion is: 45°C.

[0053] The nanoemulsion size of the nanoemulsion is: 45 nm.

[0054] Aluminum foil composite film bag for canning, filling volume 5g / bag

[0055] The appearance, color and stability of the prepared fucoxanthin nanoemulsion showed that the appearance was orange-yellow with uniform color. The nanoemulsion particle size was 45 nm. The nanoemulsion was centrifuged at a speed of 3000 r / min for 2 min. The emulsion was stable and did not stratify, with good stability.

[0056] The product taste was evaluated based on the ratio of this embodiment and the existing fucoxanthin tablets and fucoxanthin hard capsules, and the evaluation results are shown in Table 1 below:

[0057] Example Negative reviews Medium review good excellent 1 √ 2 √ tablet √ Hard Capsules √

[0058] Table 1 Product taste evaluation table

[0059] According to the results in Table 1, combined with the ratio of the fucoxanthin nano solvent in the specific embodiment 1, multiple groups of experiments with different raw material ratios and ratios as in the embodiment 2 were carried out in sequence, and the results were close to those in the above Table 1. The taste evaluation of the obtained fucoxanthin nano solvents was good or excellent, which was better than the fucoxanthin tablets and fucoxanthin hard capsules. Specific embodiment three:

[0061] like Figure 1 As shown, the prepared fucoxanthin nanoemulsion was tested in a pH 6.8 solution. The experimental chart is as follows Figure 2 As shown:

[0062] in, Figure 2 The horizontal direction is the reaction time, and the vertical direction is the dissolution percentage, wherein the green line is the fucoxanthin tablet, the red line is the fucoxanthin hard capsule, and the other color lines are the fucoxanthin nanoemulsions of the present application at different ratios;

[0063] In a solution of pH 6.8, fucoxanthin nanoemulsion is 100% dissolved in 5 minutes, fucoxanthin tablets are only 5% dissolved in the 5th minute in a solution of pH 6.8, and the dissolution rate of fucoxanthin hard capsules in the 5th minute is 0 in a solution of pH 6.8. The dissolution rate of tablets and capsules at the 60th minute and the dissolution rate of nanoemulsion at the 5th minute are close to 100%. The dissolution rate of nanoemulsion is 12 times that of tablets and capsules.

[0064] In summary, the present application increases the solubility of fucoxanthin, removes the unpleasant odor of fucoxanthin, reduces gastrointestinal degradation, improves bioavailability, achieves controlled release and absorption of fucoxanthin, and has an excellent taste. The nanoemulsion in a liquid state has greatly improved the compliance of the product for women with dysphagia and middle-aged and elderly people.

[0065] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the statement "comprising a reference structure" do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0066] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a fucoxanthin nanoemulsion, characterized in that: The preparation method is as follows: Sp1: Preparation of aqueous phase: Take resistant dextrin, isomaltooligosaccharide, fructooligosaccharide, blood orange powder, L-arabinose, esterified vitamin C, citric acid, kelp polysaccharide, mono- and di-glycerol fatty acid esters, sodium octenyl succinate starch raw materials, add water to the raw materials, heat, stir, dissolve and disperse to obtain a premix liquid aqueous phase; Sp2: Preparation of oil phase: Take fucoxanthin and medium-chain triglyceride raw materials, stir, dissolve and disperse them to obtain a premix liquid oil phase; Sp3: Preparation of ultrafine suspension emulsion, the water phase and oil phase prepared by Sp1 and Sp2 are added in proportion and processed by colloid mill twice to obtain ultrafine suspension emulsion; Sp4: Preparation of fucoxanthin nanoemulsion. The ultrafine suspension emulsion in Sp3 is added into a vacuum emulsification shearing tank, and after vacuum stirring, emulsification shearing, degassing and canning, the fucoxanthin nanoemulsion is obtained.

2. The method for preparing a fucoxanthin nanoemulsion according to claim 1, characterized in that: The mass percentages of the raw materials of each component in the preparation of the aqueous phase are 5%-15% resistant dextrin, 10%-30% isomaltooligosaccharide, 10%-30% fructooligosaccharide, 1%-5% blood orange powder, 5%-10% L-arabinose, 0.5%-1.0% esterified vitamin C, 0.05%-0.2% citric acid, 1%-2% kelp polysaccharide, 0.05-0.5% mono- and di-glycerol fatty acid esters, 0.05%-0.5% sodium starch glycolate octenylsuccinate, and 15%-25% purified water raw material.

3. The method for preparing a fucoxanthin nanoemulsion according to claim 1, characterized in that: During the preparation of the water phase, the heating temperature is 65° C.-85° C., and the stirring, dissolving and dispersing time is 15 min-30 min.

4. The method for preparing a fucoxanthin nanoemulsion according to claim 1, characterized in that: The mass percentages of the raw materials of each component in the preparation of the oil phase are 0.2%-2% fucoxanthin and 10%-40% medium-chain triglycerides, respectively. The temperature environment during stirring is room temperature ≤37° C., and the stirring and mixing time is 5 min-10 min.

5. The method for preparing a fucoxanthin nanoemulsion according to claim 1, characterized in that: In the preparation of the ultrafine suspension emulsion, the ratio of the water phase to the oil phase is 3:2-9:1, the rotation speed of the colloid mill is 3000-5000 r / min, and the number of colloid mill cycles is 1-3 times.

6. The method for preparing a fucoxanthin nanoemulsion according to claim 1, characterized in that: In the preparation of the fucoxanthin nanoparticles, the shear rate of vacuum emulsification is 6000 r / min-11000 r / min, and the shear time of vacuum emulsification is 15 min-30 min.

7. The method for preparing a fucoxanthin nanoemulsion according to claim 1, characterized in that: In the preparation of the fucoxanthin nanoparticles, the vacuum degree of vacuum emulsification is 0.09-0.1 MPa, the canning temperature is 37° C.-46° C., and the size of the nanoemulsifier is 1-100 nm.

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