CN115558151A - Aerogel taking mung bean protein and burdock nanocellulose as template for synergistically stabilizing foam - Google Patents

Aerogel taking mung bean protein and burdock nanocellulose as template for synergistically stabilizing foam Download PDF

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CN115558151A
CN115558151A CN202211026457.0A CN202211026457A CN115558151A CN 115558151 A CN115558151 A CN 115558151A CN 202211026457 A CN202211026457 A CN 202211026457A CN 115558151 A CN115558151 A CN 115558151A
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burdock
nanocellulose
aerogel
mung bean
fiber
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CN115558151B (en
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李莹
冯进
吴彤
柴智
马恺扬
胡昕迪
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Baima Future Food Research Institute
Jiangsu Academy of Agricultural Sciences
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Baima Future Food Research Institute
Jiangsu Academy of Agricultural Sciences
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/12Ketones
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • A61K47/38Cellulose; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/42Proteins; Polypeptides; Degradation products thereof; Derivatives thereof, e.g. albumin, gelatin or zein
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/06Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2205/00Foams characterised by their properties
    • C08J2205/02Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
    • C08J2205/026Aerogel, i.e. a supercritically dried gel
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2205/00Foams characterised by their properties
    • C08J2205/04Foams characterised by their properties characterised by the foam pores
    • C08J2205/042Nanopores, i.e. the average diameter being smaller than 0,1 micrometer
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2301/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/02Cellulose; Modified cellulose
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2389/00Characterised by the use of proteins; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2401/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2401/02Cellulose; Modified cellulose
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2489/00Characterised by the use of proteins; Derivatives thereof

Abstract

The invention relates to an aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as a template, which comprises the following steps: selecting fresh burdock as a raw material, cleaning, drying, carrying out superfine grinding and sieving, mixing and stirring burdock fine powder and water uniformly, adding amylase, saccharifying enzyme and papain respectively, boiling in water bath to inactivate enzymes, and centrifuging to obtain the burdock fiber. Washing the obtained burdock fiber for multiple times, centrifuging to remove trace impurities to obtain a fiber solution, freeze-drying the fiber solution to obtain burdock fiber powder, dispersing the burdock fiber powder in a sodium citrate buffer solution containing xylanase and cellulase, boiling to inactivate the enzyme after stirring, centrifuging after ultrasonic treatment, collecting precipitate, and washing the precipitate with absolute ethyl alcohol to obtain the burdock nanocellulose. Homogenizing burdock nanocellulose and mung bean protein to form foam. And (4) putting the foam into a refrigerator for freeze drying to obtain the aerogel. Compared with the prior aerogel, the burdock used as the raw material has low cost and is easy to obtain, and the cost of the aerogel can be reduced.

Description

Aerogel taking mung bean protein and burdock nanocellulose as template for synergistically stabilizing foam
Technical Field
The invention relates to aerogel taking mung bean protein and burdock nanocellulose as a template for synergistically stabilizing foam, and belongs to the technical field of aerogel biotechnology.
Background
Although the planting area of the burdock is wide in China, the domestic utilization rate of the burdock is not high, the research and development of deep products are lacked, and the waste of the existing burdock resources is caused to a great extent. The burdock root as the main edible part of the burdock contains rich dietary fiber, the burdock has the most dietary fiber content in root plants, has the advantages of complete biodegradation, easy modification, good biocompatibility and the like, and can be used for preparing finer nano cellulose through finish machining.
The aerogel is a novel functional material, is a porous solid, has nanoscale pore channels distributed on the surface, and has high porosity and large specific surface area, and the excellent porosity and specific surface area provide structural support for the aerogel in the fields of food, medicine, bioscience, adsorption and the like. The three-dimensional pore structure of the aerogel can play a role in slow release in the fields of loading active substances and drug delivery, and has good application prospect.
However, the conventional aerogel price is manufactured by using chemical substances manually, so that the conventional aerogel price is expensive and high in cost, and more different raw materials are needed to solve the problem.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the existing problems and defects, the invention aims to provide the aerogel taking mung bean protein and burdock nanocellulose as the template and being a white spongy porous solid with good mechanical property and adsorbability. The mung bean protein is mixed to form a new composite material, so that the biocompatibility of the burdock nanocellulose is improved, and meanwhile, the strength of the burdock nanocellulose and mung bean protein aerogel composite material is improved by using the high-strength nanostructure of the burdock nanocellulose. Can be used for exploring the application of the aerogel material taking the foam as the template in the aspects of structured grease, functional factor targeted delivery and the like. Compared with the currently used aerogel, the burdock serving as the raw material is low in cost and easy to obtain, and the cost of the aerogel can be reduced.
The technical scheme is as follows: in order to realize the purpose, the invention adopts the following technical scheme:
an aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as a template is characterized in that: the method comprises the following steps:
step 1: pretreatment of raw materials: selecting fresh burdock as a raw material, cleaning, drying, carrying out superfine grinding and sieving to obtain burdock fine powder;
step 2: preparing burdock fiber: mixing the burdock fine powder obtained in the step 1 with water, stirring uniformly, adding amylase, glucoamylase and papain respectively, boiling in a water bath to inactivate enzymes, and centrifuging to obtain burdock fiber;
and step 3: preparing burdock fiber powder: washing and centrifuging the burdock fiber obtained in the step 2 for many times to remove trace impurities to obtain a fiber solution, and freeze-drying the fiber solution to obtain burdock fiber powder;
and 4, step 4: preparing burdock nanocellulose: dispersing the burdock fiber powder obtained in the step 3 in a sodium citrate buffer solution containing xylanase and cellulase, boiling to inactivate the enzyme after stirring, centrifuging after ultrasonic treatment, collecting precipitate, and cleaning the precipitate with absolute ethyl alcohol to obtain burdock nanocellulose;
and 5: homogenizing the burdock nanocellulose obtained in the step (4) and the mung bean protein to form foam;
step 6: and (5) putting the foam obtained in the step (5) into a refrigerator for freeze drying to obtain the aerogel.
Further, the mixture is subjected to superfine grinding in the step 1 until the particle size is 20-40 μm, and the mixture is sieved by a sieve with 400-600 meshes.
Further, in the step 2, the burdock fine powder and water are mixed according to the mass ratio of 1.
Further, centrifuging at the rotating speed of 5000 g/min for 10 to 25min in the step 2 to obtain the burdock fiber.
Further, a magnetic stirrer is used for stirring uniformly in the step 2.
Further, washing is performed using water and ethanol in the step 3.
Further, in the step 4, 50 mM sodium citrate buffer solution containing 2000U/mL xylanase and 3000U/mL cellulase is used, burdock fiber powder and the sodium citrate buffer solution are prepared according to the mass ratio of 1.
Further, in the step 5, 1% of burdock nanocellulose and 10% of mung bean protein are used.
Further, in the step 5, a homogenizer is used for homogenizing at 8000rpm for 10-20min to form foam.
Further, the temperature of the refrigerator in the step 6 is-60 to-100 ℃.
Has the advantages that: compared with the prior art, the novel aerogel taking the mung bean protein and burdock nanocellulose synergistic stable foam as the template has the following advantages: has high porosity, and can be loaded with active substances and has sustained release effect. The burdock and mung bean food has high safety, is green and healthy, and has high value. The burdock is economical and practical, has stable source and is easy to realize industrialized development. The aerogel prepared by the method is a white spongy porous solid, the surface of the aerogel is covered with nanoscale pore channels, the porosity is high, the aerogel has good adsorbability and reusability, and the aerogel has a good slow release effect after being loaded with curcumin.
Drawings
FIG. 1 is a schematic of a homogeneous foam of an embodiment of the present invention;
FIG. 2 is a diagram of aerogel preparation according to an embodiment of the present invention;
FIG. 3 is a scanning electron micrograph of an aerogel according to an embodiment of the present invention;
figure 4 is a diagram of a finished curcumin oleogel preparation of an embodiment of the present invention;
fig. 5 is a simulated hydrolysis diagram of in vitro digestion of curcumin aerogel in accordance with an embodiment of the present invention.
Detailed Description
The present invention is further illustrated by the following detailed description in conjunction with the accompanying drawings, it is to be understood that such embodiments are merely illustrative of and not restrictive on the broad invention, and that various equivalent modifications of the invention may occur to those skilled in the art upon reading the appended claims.
An aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as a template comprises the following specific steps:
(1) Preparation of burdock nano-cellulose
a: selecting burdock raw materials: selecting fresh burdock with the diameter of 4-6 cm as a raw material;
b: pretreatment of an extracted sample: washing burdock, drying, micronizing to obtain particles with a particle size of about 20 to 40 mu m, and sieving with a sieve of 400 to 600 meshes to obtain burdock fine powder;
c: preparing burdock nanocellulose: mixing the obtained 100 g of burdock powder with 500 mL of water, and uniformly dispersing by using a magnetic stirrer; respectively adding 0.15g alpha-amylase (60 deg.C, pH 4.5) for treating for 40 min,0.20 g saccharifying enzyme (60 deg.C, pH 6.0) for treating for 40 min,1.0 g papain (50 deg.C, pH 6.0) for treating for 60 min, and boiling in water bath to inactivate enzyme. Centrifuging at 5000 g/min for 5-20 min to obtain burdock fiber as light grey precipitate, washing with water and ethanol for several times, centrifuging to remove trace impurities to obtain fiber solution, and lyophilizing to obtain powdery fiber material. Dispersing 5g of burdock fiber powder in 250 mL of sodium citrate buffer (50 mM, pH 4.8) containing xylanase (2000U/mL) and cellulase (3000U/mL), and stirring for 18-30 h at 50 ℃ for 600 r/min; then boiling the sample for 5 to 15min to inactivate enzyme, carrying out ultrasonic treatment for 1 to 3h at 600W, centrifuging for 5 to 15min at 1000 g/min, collecting precipitate, and repeating twice; washing the precipitate with anhydrous ethanol, repeating twice, and collecting precipitate which is burdock nanocellulose separated from burdock fiber.
(2) Homogenizing the burdock nanocellulose obtained in the step (1) by a homogenizer at 8000rpm for 15min according to the concentration of 1% and the mung bean protein with the concentration of 10%, and forming rich foam after homogenization;
(3) And (3) putting the foam obtained in the step (2) into a refrigerator at-60 to-100 ℃, and freeze-drying to prepare the aerogel.
Example 1
(1) Preparation of burdock nano-cellulose
a: selecting burdock raw materials: selecting fresh burdock with the diameter of 5cm as a raw material;
b: pretreatment of an extracted sample: washing burdock, drying, micronizing to obtain particle size of about 30 μm, and sieving with 600 mesh sieve to obtain burdock fine powder;
c: preparing burdock nanocellulose: mixing 100 g of the obtained burdock powder with 500 mL of water, and uniformly dispersing by using a magnetic stirrer; respectively adding 0.15g alpha-amylase (60 deg.C, pH 4.5) for treatment for 40 min,0.20 g diastase (60 deg.C, pH 6.0) for treatment for 40 min,1.0 g papain (50 deg.C, pH 6.0) for treatment for 60 min, boiling in water bath to inactivate enzyme. Centrifuging at 5000 g/min for 10 min to obtain Burdock fiber as light grey precipitate, washing with water and ethanol for several times, centrifuging to remove trace impurities to obtain fiber solution, and lyophilizing to obtain powdery fiber material. Dispersing 5g of burdock fiber powder in 250 mL of sodium citrate buffer (50 mM, pH 4.8) containing xylanase (2000U/mL) and cellulase (3000U/mL), stirring at 50 ℃ for 24 h at 600 r/min; then boiling the sample for 10 min to inactivate enzyme, carrying out ultrasonic treatment at 600W for 2.0 h, centrifuging at 1000 g/min for 10 min, collecting precipitate, and repeating twice; washing the precipitate with anhydrous ethanol, repeating twice, and collecting precipitate which is burdock nano-cellulose separated from burdock fiber.
(2) As shown in figure 1, the obtained burdock nanocellulose is homogenized for 15min at the concentration of 1% and the mung bean protein with the concentration of 10% by using a homogenizer at 8000rpm, rich foam is formed after homogenization, and the foam can be maintained for 47 h at normal temperature.
(3) As shown in figure 2, the aerogel is prepared by placing the foam formed by homogenizing mung bean protein and burdock nanocellulose into a refrigerator at the temperature of 80 ℃ below zero, and freeze-drying. The state of the aerogel in an electron microscope is shown in FIG. 3.
(4) As shown in fig. 4, under the heating condition of 80 ℃, the corn oil with 1% curcumin in the loading capacity is dissolved, the aerogel adsorbs the corn oil with curcumin dissolved, and the mass ratio of the curcumin oil solution to the aerogel is 5.
In vitro digestion simulation of curcumin-loaded oleogels, results are shown in figure 5. Preparation of gastric digestive juice: 2 mg/mL NaCl, 7 mL/L HCI and 3.2 mg/mL pepsin, wherein all the components are prepared by ultrapure water; preparation of intestinal juice: salt solution (36.7 mg/mL CaC 1) 2 . H 2 O, 218.7 mg/mL NaCI), 24 mg/mL lipase, 54 mg/mL bile salt, where the salt solution was formulated with ultrapure water, and the lipase and bile salt were formulated with 5 mmol/L PBS (pH 7.0). Preheating the gastric digestive juice at 37 ℃ for 5min, taking 15 ml, adding 15g of curcumine oleogel, quickly adjusting the pH value of the mixed system to 2.5 by using 1 mol/L NaOH, digesting in a constant-temperature shaker water bath (100 r/min) at 37 ℃ for 2 h, and quickly adjusting the pH value of the mixed system to 7.0 by using 2 mol/L NaOH after the gastric digestion is finished. Preheating the intestinal mimic solution at 37 ℃ for 5min, sequentially adding 1.5 mL of salt solution, 3.5mL of cholate solution and 2.5mL of lipase solution into the gastric digestive juice, adjusting the pH of the mixed system to 7.0 by using 1 mol/L NaOH, and finally digesting in 37 ℃ constant-temperature shaking table water bath (100 r/min) for 2 h. During the process, naOH is continuously used for adjusting so that the pH value of the mixed system is maintained at 7.0. The amount of free fatty acids that are hydrolyzed by lipase in the sample during simulated digestion in vitro is measured.
FFA release rate (%) =100 × C NaOH ×V NaOH ×M×2W
In the formula, C NaOH Is the molar concentration of NaOH solution used for titration;
m is the mass fraction of corn oil (872 g/mol);
w is the weight (g) of corn oil during digestion.
Therefore, the aerogel disclosed by the invention can achieve a better slow release effect, has a similar effect to that of an ordinary aerogel, and is lower in cost.

Claims (9)

1. An aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as a template is characterized in that: the method comprises the following steps:
step 1: pretreatment of raw materials: selecting fresh burdock as a raw material, cleaning, drying, carrying out superfine grinding and sieving to obtain burdock fine powder;
step 2: preparing burdock fiber: mixing the burdock fine powder obtained in the step 1 with water, uniformly stirring, respectively adding amylase, glucoamylase and papain, boiling in a water bath to inactivate enzymes, and centrifuging to obtain burdock fiber;
and 3, step 3: preparing burdock fiber powder: washing and centrifuging the burdock fiber obtained in the step 2 for many times to remove trace impurities to obtain a fiber solution, and freeze-drying the fiber solution to obtain burdock fiber powder;
and 4, step 4: preparing burdock nanocellulose: dispersing the burdock fiber powder obtained in the step 3 in a sodium citrate buffer solution containing xylanase and cellulase, boiling to inactivate the enzyme after stirring, centrifuging after ultrasonic treatment, collecting precipitate, and cleaning the precipitate with absolute ethyl alcohol to obtain burdock nanocellulose;
and 5: homogenizing the burdock nanocellulose obtained in the step (4) and the mung bean protein to form foam;
step 6: and (5) putting the foam obtained in the step (5) into a refrigerator for freeze drying to obtain the aerogel.
2. The aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as a template as claimed in claim 1, is characterized in that: the superfine powder in the step 1 is crushed to a particle size of 20 to 40 mu m and sieved by a sieve of 400 to 600 meshes.
3. The aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as a template as claimed in claim 1, is characterized in that: in the step 2, the burdock fine powder and water are mixed according to the mass ratio of 1 to 5 to obtain a mixed solution, and the mass ratio of the added amylase, the saccharifying enzyme and the papain to the mixed solution is (2 to 4): 3 to 5): 19 to 21): 12000.
4. The aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as a template as claimed in claim 1, is characterized in that: and (3) centrifuging at the rotating speed of 5000 g/min for 10 to 25min in the step 2 to obtain the burdock fiber.
5. The aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as the template according to claim 1 is characterized in that: and (3) uniformly stirring by using a magnetic stirrer in the step (2), and washing by using water and ethanol in the step (3).
6. The aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as a template as claimed in claim 1, is characterized in that: in the step 4, 50 mM sodium citrate buffer solution containing 2000U/mL xylanase and 3000U/mL cellulase is used, burdock fiber powder and the sodium citrate buffer solution are prepared according to the mass ratio of 1 to 50, the mixture is stirred for 18 to 30h at the temperature of 20 to 80 ℃ and is boiled for 5 to 15min to inactivate enzyme, ultrasonic treatment is carried out for 1 to 3h at 600W, and the mixture is centrifuged for 5 to 15min at 1000 g/min.
7. The aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as a template as claimed in claim 1, is characterized in that: in the step 5, 1% of burdock nanocellulose and 10% of mung bean protein are used.
8. The aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as a template as claimed in claim 1, is characterized in that: and 5, homogenizing at 8000rpm for 10-20min by using a homogenizer to form foam.
9. The aerogel taking mung bean protein and burdock nanocellulose synergistic stable foam as the template according to claim 1 is characterized in that: the temperature of the refrigerator in the step 6 is-60 to-100 ℃.
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