CN113367323A - Green preparation method of food-grade multifunctional lignin/silicon dioxide nanoparticle emulsifier - Google Patents

Green preparation method of food-grade multifunctional lignin/silicon dioxide nanoparticle emulsifier Download PDF

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CN113367323A
CN113367323A CN202110674614.8A CN202110674614A CN113367323A CN 113367323 A CN113367323 A CN 113367323A CN 202110674614 A CN202110674614 A CN 202110674614A CN 113367323 A CN113367323 A CN 113367323A
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lignin
water
food
emulsifier
green preparation
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陈凯
戚栋明
陈凤凤
袁胜荣
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Zhejiang University of Technology ZJUT
Zhejiang Sci Tech University ZSTU
Zhejiang University of Science and Technology ZUST
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, 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
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/10—Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/02—Inorganic compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25—Silicon; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04—Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention discloses a green preparation method of a food-grade multifunctional lignin/silicon dioxide nanoparticle emulsifier, which comprises the steps of dissolving enzymatic lignin in a sodium hydroxide aqueous solution, centrifuging to remove incompatible impurities, adjusting the pH to be neutral, centrifuging again to remove water-insoluble lignin, dialyzing, freeze-drying to obtain water-soluble lignin for later use, weighing SiO2Dispersing the nanoparticles in water, adding chitosan solution, stirring for a period of timeThen centrifuging to remove supernatant, washing the residual solid with ultrapure water, dispersing the particles in water again, adding the water-soluble lignin, stirring, centrifuging to remove supernatant, washing the residual solid with ultrapure water, and freeze-drying to obtain a final sample2Application potential in the food field.

Description

Green preparation method of food-grade multifunctional lignin/silicon dioxide nanoparticle emulsifier
Technical Field
The invention relates to the field of emulsifier preparation, and in particular relates to a green preparation method of a food-grade multifunctional lignin/silicon dioxide nanoparticle emulsifier.
Background
Curcumin is a hydrophobic polyphenol extracted from the rhizome of the turmeric plant, and accounts for about 3 wt.% of the dry weight of the material. Due to the existence of a ketone/enol structure and two phenolic groups in the molecular structure of curcumin, the curcumin has good pharmacological effects of anti-inflammation, oxidation resistance, tumor resistance, aging resistance and the like, and has great application potential in the fields of medicines, cosmetics, functional foods and the like. According to statistics, the global curcumin market value in 2017 is about 5245 million dollars, and with the diversification of application fields, the global curcumin market scale is expected to reach 1.519 million dollars by 2027. However, the problems of short shelf life due to chemical instability and poor bioavailability due to low water solubility of curcumin still limit the large-scale application of curcumin in the fields of food, cosmetics, medicine and the like.
Emulsions are widely used in food, pharmaceutical and cosmetic processing and in the final consumer products as soft templates or carriers for nutritional ingredients. Among them, High Internal Phase Emulsions (HIPEs) are attracting attention in the fields of food, medicine, cosmetics, and the like due to their advantages of high drug loading due to their ultra-high internal phase volume (not less than 74%), adjustable rheological properties, and the like. Furthermore, HIPEs can directly convert liquid oil phases into solid fats, and are one of the ideal substitutes for hydrogenated oils (PHOs). And secondly, the oil-in-water HIPEs can effectively prevent the breeding of microorganisms due to low water content, and have longer shelf life compared with other emulsion systems. The preparation of conventional HIPEs usually requires a large amount of small molecule surfactants (5-50 wt%) such as APG and SDS, and the use of small molecule surfactants in the fields of food, biomedicine and cosmetics is increasingly limited as the requirements of green, safe, non-toxic, biocompatible and biodegradable increase by consumers and laws.
Amorphous silica nanoparticles (SiO)2NPs) have been registered and approved by the European Union (EU) and the US (US) as E551 food additives, commonly used as glidants or stabilizers in food products, e.g. to stabilize water-in-oil emulsions in chocolate confectionery. Furthermore, SiO2NPs stabilize emulsion droplet sizes on the order of microns or even sub-microns, which is typical droplet size needed to improve food appearance and stability. However, as a stabilizer for HIPEs, SiO2The surface properties of the NPs need to be further adjusted to obtain the appropriate degree of hydrophobicity to ensure optimal wettability at the oil-water interface. At present, researchers have succeeded in preparing a variety of amphiphilic SiO through a chemical grafting strategy2NPs and intelligent HIPEs are constructed, but the toxicity and biocompatibility of the new compound need to be further researched, and the large-scale application of the new compound in the fields of food, cosmetics, medicines and the like is limited. Bismarck et al hydrophobized SiO by adsorption of oleic acid2NPs, constructed internal phase volumes up to 92 vol% HIPEs. However, such HIPEs lack uv oxidation protection properties, making the active substances loaded therein susceptible to deterioration, even toxicity.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide food-grade multifunctional lignin/SiO2A green preparation method of a nano-particle emulsifier.
The invention also aims to provide the lignin/SiO2A method for preparing stable high internal phase emulsion and an optimal formula.
The invention further aims to provide a lignin/SiO-based material2Use of a stable high internal phase emulsion in the emulsion field.
The purpose of the invention is realized by the following scheme: a green preparation method of a food-grade multifunctional lignin/silicon dioxide nanoparticle emulsifier is characterized in that reaction raw materials comprise enzymatic hydrolysis lignin, chitosan and nano SiO2。
Preferably, the preparation process comprises the following steps:
s1, dissolving the enzymatic hydrolysis lignin in a sodium hydroxide aqueous solution, centrifuging to remove incompatible impurities, adjusting the pH value to be neutral, centrifuging again to remove water-insoluble lignin, dialyzing, and freeze-drying to obtain water-soluble lignin for later use;
s2, weighing SiO2Dispersing nano particles in water, adding a chitosan solution, stirring for a period of time, centrifuging to remove a supernatant, washing the residual solid with ultrapure water, dispersing the particles in water again, adding the water-soluble lignin, stirring, centrifuging to remove the supernatant, washing the residual solid with ultrapure water, and freeze-drying to obtain the final sample.
Preferably, the concentration of the enzymatic hydrolysis lignin added in the step S2 is 15-25 wt%.
Preferably, the concentration of the chitosan solution in the step S2 is 5-20 g/mL.
Preferably, the silica has a mass of 2 to 8g in the step S2.
Preferably, the water-soluble lignin is added in the step S2 in an amount of 0.5-20g by mass.
Preferably, the molecular weight of the dialysis bag in the step S2 is Mw 3000 Da.
A preparation method of stable high internal phase emulsion comprises the steps of using the nanoparticle emulsifier prepared by any method, weighing the nanoparticle emulsifier prepared by any method, dispersing in water, adding soybean oil, and carrying out high-speed shearing emulsification to construct HIPEs food emulsion.
Preferably, the soybean oil is added in an amount of 75 to 90 vol%.
Preferably, the emulsifier is weighed in an amount of 0.1 to 1.5 g.
Has the advantages that:
compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention creatively and environmentally synthesizes multifunctional food-grade lignin/SiO from bioethanol enzymolysis residues2The nano particles are used for constructing HIPEs, a new method is provided for green preparation of the multifunctional food-grade emulsifier, and wood is expandedElemental and SiO2Application potential in the food field.
2. The ingenious structural combination of lignin and silicon dioxide can promote SiO2The emulsifying activity of the NPs can endow the NPs with good ultraviolet oxidation resistance, and food-grade SiO is expanded2NPs have potential application in the fields of biological medicine, cosmetics, food and the like.
Drawings
FIG. 1 a macroscopic digital photograph and microstructure of the high internal phase emulsion;
FIG. 2 is a schematic diagram of food grade multifunctional lignin/silica nanoparticle preparation;
figure 3 graph of simulated digestion performance of high internal phase emulsions in vitro.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
Example 1
4.0g of enzymatically hydrolyzed lignin was dissolved in 20mL of a 1mol/L aqueous solution of sodium hydroxide and centrifuged to remove incompatible impurities. Then, the pH was adjusted to neutral with 0.1mol/L hydrochloric acid solution, and the water-insoluble lignin was removed by centrifugation again, dialyzed, and freeze-dried for use. 2.0g of SiO are weighed2Dispersing the nanoparticles in 10mL of pure water, adding 1mL of 5g/mL chitosan solution, stirring for 10min, centrifuging to remove the supernatant, and washing the remaining solid with ultrapure water for 2 times. Then, dispersing the above particles in pure water again, adding 0.5g of the above water-soluble lignin, stirring for 10min, centrifuging to remove supernatant, washing the remaining solids with ultrapure water for 2 times, and freeze drying to obtain food-grade multifunctional lignin/silicon dioxide nanometerAnd (3) granules.
Example 2
4.0g of enzymatically hydrolyzed lignin was dissolved in 20mL of a 1mol/L aqueous solution of sodium hydroxide and centrifuged to remove incompatible impurities. Then, the pH was adjusted to neutral with 0.1mol/L hydrochloric acid solution, and the water-insoluble lignin was removed by centrifugation again, dialyzed, and freeze-dried for use. Weighing 4.0g of SiO2Dispersing the nanoparticles in 10mL of pure water, adding 1mL of 5g/mL chitosan solution, stirring for 10min, centrifuging to remove the supernatant, and washing the remaining solid with ultrapure water for 2 times. And then, dispersing the particles in pure water again, adding 0.5g of the water-soluble lignin, stirring for 10min, centrifuging to remove supernatant, washing the residual solid with ultrapure water for 2 times, and freeze-drying to obtain the final sample which is the food-grade multifunctional lignin/silicon dioxide nanoparticles.
Embodiment 3
4.0g of enzymatically hydrolyzed lignin was dissolved in 20mL of a 1mol/L aqueous solution of sodium hydroxide and centrifuged to remove incompatible impurities. Then, the pH was adjusted to neutral with 0.1mol/L hydrochloric acid solution, and the water-insoluble lignin was removed by centrifugation again, dialyzed, and freeze-dried for use. 6.0g of SiO are weighed2Dispersing the nanoparticles in 10mL of pure water, adding 1mL of 5g/mL chitosan solution, stirring for 10min, centrifuging to remove the supernatant, and washing the remaining solid with ultrapure water for 2 times. And then, dispersing the particles in pure water again, adding 0.5g of the water-soluble lignin, stirring for 10min, centrifuging to remove supernatant, washing the residual solid with ultrapure water for 2 times, and freeze-drying to obtain the final sample which is the food-grade multifunctional lignin/silicon dioxide nanoparticles.
Example 4
4.0g of enzymatically hydrolyzed lignin was dissolved in 20mL of a 1mol/L aqueous solution of sodium hydroxide and centrifuged to remove incompatible impurities. Then, the pH was adjusted to neutral with 0.1mol/L hydrochloric acid solution, and the water-insoluble lignin was removed by centrifugation again, dialyzed, and freeze-dried for use. 8.0g of SiO are weighed2Dispersing the nanoparticles in 10mL of pure water, adding 1mL of 5g/mL chitosan solution, stirring for 10min, centrifuging to remove the supernatant, and washing the remaining solid with ultrapure water for 2 times. Subsequently, the above particles are dispersed again in pure water,adding 0.5g of the water-soluble lignin, stirring for 10min, centrifuging to remove supernatant, washing the residual solid with ultrapure water for 2 times, and freeze-drying to obtain the final sample which is the food-grade multifunctional lignin/silicon dioxide nanoparticles.
Example 5
4.0g of enzymatically hydrolyzed lignin was dissolved in 20mL of a 1mol/L aqueous solution of sodium hydroxide and centrifuged to remove incompatible impurities. Then, the pH was adjusted to neutral with 0.1mol/L hydrochloric acid solution, and the water-insoluble lignin was removed by centrifugation again, dialyzed, and freeze-dried for use. 2.0g of SiO are weighed2Dispersing the nanoparticles in 10mL of pure water, adding 1mL of 10g/mL chitosan solution, stirring for 10min, centrifuging to remove the supernatant, and washing the remaining solid with ultrapure water for 2 times. And then, dispersing the particles in pure water again, adding 0.5g of the water-soluble lignin, stirring for 10min, centrifuging to remove supernatant, washing the residual solid with ultrapure water for 2 times, and freeze-drying to obtain the food-grade multifunctional lignin/silicon dioxide nanoparticles.
Example 6
4.0g of enzymatically hydrolyzed lignin was dissolved in 20mL of a 1mol/L aqueous solution of sodium hydroxide and centrifuged to remove incompatible impurities. Then, the pH was adjusted to neutral with 0.1mol/L hydrochloric acid solution, and the water-insoluble lignin was removed by centrifugation again, dialyzed, and freeze-dried for use. 2.0g of SiO are weighed2Dispersing the nanoparticles in 10mL of pure water, adding 1mL of 15g/mL chitosan solution, stirring for 10min, centrifuging to remove the supernatant, and washing the remaining solid with ultrapure water for 2 times. And then, dispersing the particles in pure water again, adding 0.5g of the water-soluble lignin, stirring for 10min, centrifuging to remove supernatant, washing the residual solid with ultrapure water for 2 times, and freeze-drying to obtain the final sample which is the food-grade multifunctional lignin/silicon dioxide nanoparticles.
Example 7
4.0g of enzymatically hydrolyzed lignin was dissolved in 20mL of a 1mol/L aqueous solution of sodium hydroxide and centrifuged to remove incompatible impurities. Then, the pH was adjusted to neutral with 0.1mol/L hydrochloric acid solution, and the water-insoluble lignin was removed by centrifugation again, dialyzed, and freeze-dried for use. Weighing 2.0gSiO2Nanoparticles are dispersed in 101mL of 20g/mL chitosan solution was added to mL of pure water, and after stirring for 10min, the supernatant was removed by centrifugation, and the remaining solid was washed with ultrapure water 2 times. And then, dispersing the particles in pure water again, adding 0.5g of the water-soluble lignin, stirring for 10min, centrifuging to remove supernatant, washing the residual solid with ultrapure water for 2 times, and freeze-drying to obtain the final sample which is the food-grade multifunctional lignin/silicon dioxide nanoparticles.
Example 8
4.0g of enzymatically hydrolyzed lignin was dissolved in 20mL of a 1mol/L aqueous solution of sodium hydroxide and centrifuged to remove incompatible impurities. Then, the pH was adjusted to neutral with 0.1mol/L hydrochloric acid solution, and the water-insoluble lignin was removed by centrifugation again, dialyzed, and freeze-dried for use. Weighing 2.0gSiO2Dispersing the nanoparticles in 10mL of pure water, adding 1mL of 5g/mL chitosan solution, stirring for 10min, centrifuging to remove the supernatant, and washing the remaining solid with ultrapure water for 2 times. And then, dispersing the particles in pure water again, adding 1.0g of the water-soluble lignin, stirring for 10min, centrifuging to remove supernatant, washing the residual solid with ultrapure water for 2 times, and freeze-drying to obtain the final sample which is the food-grade multifunctional lignin/silicon dioxide nanoparticles.
Example 9
4.0g of enzymatically hydrolyzed lignin was dissolved in 20mL of a 1mol/L aqueous solution of sodium hydroxide and centrifuged to remove incompatible impurities. Then, the pH was adjusted to neutral with 0.1mol/L hydrochloric acid solution, and the water-insoluble lignin was removed by centrifugation again, dialyzed, and freeze-dried for use. Weighing 2.0gSiO2Dispersing the nanoparticles in 10mL of pure water, adding 1mL of 5g/mL chitosan solution, stirring for 10min, centrifuging to remove the supernatant, and washing the remaining solid with ultrapure water for 2 times. And then, dispersing the particles in pure water again, adding 1.5g of the water-soluble lignin, stirring for 10min, centrifuging to remove supernatant, washing the residual solid with ultrapure water for 2 times, and freeze-drying to obtain the final sample which is the food-grade multifunctional lignin/silicon dioxide nanoparticles.
Example 10
Dissolving 4.0g of enzymatic hydrolysis lignin in 20mL of 1mol/L sodium hydroxide aqueous solution, and centrifuging to remove ligninA capacitive impurity. Then, the pH was adjusted to neutral with 0.1mol/L hydrochloric acid solution, and the water-insoluble lignin was removed by centrifugation again, dialyzed, and freeze-dried for use. 2.0g of SiO are weighed2Dispersing the nanoparticles in 10mL of pure water, adding 1mL of 5g/mL chitosan solution, stirring for 10min, centrifuging to remove the supernatant, and washing the remaining solid with ultrapure water for 2 times. And then, dispersing the particles in pure water again, adding 2.0g of the water-soluble lignin, stirring for 10min, centrifuging to remove supernatant, washing the residual solid with ultrapure water for 2 times, and freeze-drying to obtain the final sample which is the food-grade multifunctional lignin/silicon dioxide nanoparticles.
Example 11
0.1g of the example 1 food grade multifunctional lignin/SiO2The nanoparticles are dispersed in 2mL of pure water, 8mL of soybean oil is added, and the high-speed shearing emulsification is carried out to obtain the stable high internal phase emulsion. A macroscopic digital photograph and microstructure of the high internal phase emulsion is shown in figure 2.
Example 12
0.5g of the example 2 food grade multifunctional lignin/SiO2The nanoparticles are dispersed in 2mL of pure water, 8mL of soybean oil is added, and the high-speed shearing emulsification is carried out to obtain the stable high internal phase emulsion. A macroscopic digital photograph and microstructure of the high internal phase emulsion is shown in figure 2.
Example 13
1.0g of the example 3 food grade multifunctional lignin/SiO2The nanoparticles are dispersed in 2mL of pure water, 8mL of soybean oil is added, and the high-speed shearing emulsification is carried out to obtain the stable high internal phase emulsion. A macroscopic digital photograph and microstructure of the high internal phase emulsion is shown in figure 2.
Example 14
1.5g of example 4 food grade multifunctional lignin/SiO2The nanoparticles are dispersed in 2mL of pure water, 8mL of soybean oil is added, and the high-speed shearing emulsification is carried out to obtain the stable high internal phase emulsion. A macroscopic digital photograph and microstructure of the high internal phase emulsion is shown in figure 2.
Example 15
0.5g of example 5 food grade multifunctional lignin/SiO2The nanoparticles are dispersed in 1.58.5mL of soybean oil was added to mL of purified water and emulsified by high shear to obtain a stable high internal phase emulsion. A macroscopic digital photograph and microstructure of the high internal phase emulsion is shown in figure 2.
Example 16
0.5g of example 6 food grade multifunctional lignin/SiO2The nanoparticles were dispersed in 1.5mL of purified water, 8.5mL of soybean oil was added, and a stable high internal phase emulsion was obtained by high speed shear emulsification. A macroscopic digital photograph and microstructure of the high internal phase emulsion is shown in figure 2.
Example 17
0.5g of example 7 food grade multifunctional lignin/SiO2The nanoparticles were dispersed in 1.7mL of purified water, 8.3mL of soybean oil was added, and a stable high internal phase emulsion was obtained by high speed shear emulsification. A macroscopic digital photograph and microstructure of the high internal phase emulsion is shown in figure 2.
Example 18
0.5g of example 8 food grade multifunctional lignin/SiO2The nanoparticles were dispersed in 0.7mL of purified water, 8.7mL of soybean oil was added, and a stable high internal phase emulsion was obtained by high speed shear emulsification. A macroscopic digital photograph and microstructure of the high internal phase emulsion is shown in figure 2.
Example 19
0.5g of example 9 food grade multifunctional lignin/SiO2The nanoparticles were dispersed in 1.0mL of purified water, 9.0mL of soybean oil was added, and a stable high internal phase emulsion was obtained by high speed shear emulsification. A macroscopic digital photograph and microstructure of the high internal phase emulsion is shown in figure 2.
Example 20
0.3g of the sample was mixed with 30mL of 10mol/L phosphate buffer and stirred at 37 ℃ for 2 min. Then, 25mL of simulated gastric fluid was added and the pH of the solution was adjusted to 2.0 with 1.0mol/L hydrochloric acid. The mixture was incubated for 1h at 37 ℃ on a shaker at 100 rpm. Immediately, the pH of the solution was adjusted to 7.5 with 0.25mol/L sodium hydroxide solution. Subsequently, 8g of the bile salt solution and 5g of the lipase suspension were added to the above solution. Using a water phase electric potential titrator, taking 0.25mol/L sodium hydroxide as a titration solution, maintaining the pH value of the solution at 7.5 at 37 ℃, and carrying out a simulated fat decomposition process in the intestinal tract for 2 hours. The digested sample was further centrifuged at 10000rpm for 20min, 10mL of n-hexane was used to extract beta-carotene from the aqueous micelles, and the concentration was measured using an ultraviolet-visible spectrophotometer. The simulated digestion performance of the high internal phase emulsion in vitro is shown in figure 3.
Example 21
Food-grade multifunctional lignin/SiO2The nano-particle emulsifier is obtained by self-assembling the following components in parts by mass:
performing enzymolysis on lignin; chitosan; nano SiO2
The lignin/SiO2The nano-particles are prepared by a method comprising the following steps:
dissolving the enzymatic hydrolysis lignin in a sodium hydroxide aqueous solution, and centrifuging to remove incompatible impurities. Then, the pH was adjusted to neutral with a dilute hydrochloric acid solution, and the water-insoluble lignin was removed by centrifugation again, dialyzed, and freeze-dried for future use. Weighing a certain amount of SiO2Dispersing the nano particles in a certain volume of pure water, adding a certain volume of chitosan solution, stirring for a period of time, centrifuging to remove supernatant, and washing the residual solids with ultrapure water for 2 times. And then, dispersing the particles in pure water again, adding a certain mass of the water-soluble lignin, stirring for a period of time, centrifuging to remove supernatant, washing the residual solid with ultrapure water for 2 times, and freeze-drying to obtain the final sample.
The concentration of the enzymatic hydrolysis lignin solution is preferably 20 wt.%.
The molecular weight of the dialysis bag is preferably Mw 3000 Da.
The chitosan solution is preferably 5, 10, 15 and 20 g/mL.
The silica masses mentioned are preferably 2, 4, 6 and 8 g.
The mass of the water-soluble lignin is preferably 0.5, 1.0, 1.5 and 20 g.
The pH of the aqueous solution is preferably 7.0, 8.0, 9.0 and 10.0.
The invention further provides the food-grade multifunctional lignin/SiO2A method for preparing a nanoparticle stable high internal phase emulsion,the method comprises the following steps: weighing a certain amount of multifunctional lignin/SiO2Dispersing the nano particles in a certain volume of pure water, adding a certain volume of soybean oil, and carrying out high-speed shearing emulsification to construct the HIPEs food emulsion.
The soy oil volume is preferably 75, 80, 83, 85 and 90 vol%.
The multifunctional lignin/SiO2The particle masses are preferably 0.1, 0.5, 1.0 and 1.5 g.
The invention also performs an in vitro simulated digestion test of the high internal phase emulsion, comprising the following steps: simulated Gastric Fluid (SGF) preparation: 0.2g of sodium chloride and 0.32g of pepsin were added to 100mL of ultrapure water, and the pH of the solution was adjusted to 1.2 with 1.0mol/L hydrochloric acid for further use. Preparing a bile salt solution: 3.75g of bile salt was dissolved in 80mL of 10mmol/L phosphate buffer (pH 7.0) for further use. Preparing a lipase suspension: 0.6g of the buffer solution was dissolved in 50mL of 10mmol/L phosphate buffer (pH 7.0) and then stored.
0.3g of the sample was mixed with 30mL of 10mol/L phosphate buffer and stirred at 37 ℃ for 2 min. Then, 25mL of simulated gastric fluid was added and the pH of the solution was adjusted to 2.0 with 1.0mol/L hydrochloric acid. The mixture was incubated for 1h at 37 ℃ on a shaker at 100 rpm. Immediately, the pH of the solution was adjusted to 7.5 with 0.25mol/L sodium hydroxide solution. Subsequently, 8g of the bile salt solution and 5g of the lipase suspension were added to the above solution. Using a water phase electric potential titrator, taking 0.25mol/L sodium hydroxide as a titration solution, maintaining the pH value of the solution at 7.5 at 37 ℃, and carrying out a simulated fat decomposition process in the intestinal tract for 2 hours. The formula for the free fatty acids (FAAs) released after digestion of the sample is calculated as follows:
Figure BDA0003120244080000141
wherein V is the volume of sodium hydroxide consumed at different times, and the unit is mL; c is the concentration of sodium hydroxide, and the unit is mol/L; mw is the molecular weight of soybean oil, 290 g/mol; m is the soybean oil content in g of the initial sample.
The digested sample was further centrifuged at 10000rpm for 20min, 10mL of n-hexane was used to extract beta-carotene from the aqueous micelles, and the concentration was measured using an ultraviolet-visible spectrophotometer. Finally, the bioavailability of β -carotene can be calculated from the following formula:
Figure BDA0003120244080000142
in a pure water environment, the invention coats the lignin on the SiO by a layer-by-layer self-assembly technology2Food-grade multifunctional lignin/silicon dioxide nanoparticles (lignin @ SiO) are synthesized on the surface of NPs in a green way2NPs). And then, preparing stable HIPEs by using the particles as an emulsifier and utilizing a high-speed shearing method, researching the influence rule of the surface property and concentration of the particles and the oil-water ratio on the rheological property of an emulsion interface, the micro-morphology and the macro-stability, and constructing the structure-activity relationship between the particle structure and the performance. Meanwhile, the bioavailability of the model drug is calculated by simulating the digestion process of gastric juice and intestinal juice in vitro, so as to evaluate the application potential of the HIPEs in the food field. The implementation of the invention provides a new method for green preparation of the multifunctional food-grade emulsifier, and lignin and SiO2The application in the food field develops a new idea.
The mechanism of the invention is as follows:
the lignin has a conjugated structure of a molecular structure, high content of phenolic hydroxyl and phenyl, and amphipathy and ultraviolet resistance. In a pure water environment, the lignin is grafted and coated on the surface of the silicon dioxide by a layer-by-layer self-assembly technology, the process is green and pollution-free, and the national sustainable development strategy is met. At the same time, SiO can be promoted2The emulsifying activity of the NPs can endow the NPs with good ultraviolet oxidation resistance, and food-grade SiO is expanded2NPs have potential application in the fields of biological medicine, cosmetics, food and the like.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.

Claims (10)

1. A green preparation method of a food-grade multifunctional lignin/silicon dioxide nanoparticle emulsifier is characterized in that reaction raw materials comprise enzymatic hydrolysis lignin, chitosan and nano SiO2。
2. The green preparation method of the food grade multifunctional lignin/silica nanoparticle emulsifier according to claim 1, wherein the green preparation method comprises the following steps: the preparation process comprises the following steps:
s1, dissolving the enzymatic hydrolysis lignin in a sodium hydroxide aqueous solution, centrifuging to remove incompatible impurities, adjusting the pH value to be neutral, centrifuging again to remove water-insoluble lignin, dialyzing, and freeze-drying to obtain water-soluble lignin for later use;
s2, weighing SiO2Dispersing nano particles in water, adding a chitosan solution, stirring for a period of time, centrifuging to remove a supernatant, washing the residual solid with ultrapure water, dispersing the particles in water again, adding the water-soluble lignin, stirring, centrifuging to remove the supernatant, washing the residual solid with ultrapure water, and freeze-drying to obtain the final sample.
3. The green preparation method of the food grade multifunctional lignin/silica nanoparticle emulsifier according to claim 2, wherein the green preparation method comprises the following steps: the concentration of the enzymatic hydrolysis lignin added in the step S2 is 15-25 wt%.
4. The green preparation method of the food grade multifunctional lignin/silica nanoparticle emulsifier according to claim 3, wherein the green preparation method comprises the following steps: the concentration of the chitosan solution in the step S2 is 5-20 g/mL.
5. The green preparation method of the food grade multifunctional lignin/silica nanoparticle emulsifier according to any one of claims 2 to 4, wherein the green preparation method comprises the following steps: the mass of the silica in the step S2 is 2-8 g.
6. The green preparation method of the food grade multifunctional lignin/silica nanoparticle emulsifier according to claim 5, wherein the green preparation method comprises the following steps: in the step S2, the mass of the water-soluble lignin is 0.5-20 g.
7. The green preparation method of the food grade multifunctional lignin/silica nanoparticle emulsifier according to claim 6, wherein the green preparation method comprises the following steps: the molecular weight of the dialysis bag in step S2 is 3000 Da.
8. A method of preparing a stable high internal phase emulsion using the nanoparticle emulsifier prepared by the method of any one of claims 1 to 7, characterized in that: dispersing the nanoparticle emulsifier nanoparticles prepared by the method of any one of claims 1-7 in water, adding soybean oil, and emulsifying by high speed shearing to form a HIPEs food emulsion.
9. A method of preparing a stable high internal phase emulsion according to claim 8 wherein: the adding amount of the soybean oil is 75-90 vol%.
10. A process for preparing a stable high internal phase emulsion according to claim 8 or 9 wherein: the weighing amount of the emulsifier is 0.1-1.5 g.
CN202110674614.8A 2021-06-17 2021-06-17 Green preparation method of food-grade multifunctional lignin/silicon dioxide nanoparticle emulsifier Pending CN113367323A (en)

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