CN111848985A - Preparation method of dendrobium extract-nano cellulose composite hydrogel, product and application - Google Patents
Preparation method of dendrobium extract-nano cellulose composite hydrogel, product and application Download PDFInfo
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Abstract
The invention belongs to the technical field of antioxidant materials, and particularly relates to a preparation method, a product and application of a dendrobium extract-nano cellulose composite hydrogel. The preparation method comprises the following steps: cleaning fresh herba Dendrobii, air drying, cutting from the root-stem junction, and respectively preserving root and stem-leaf; taking stem and leaf parts, and preparing the stem and leaf extract of the dendrobium by adopting the steps of ethanol extraction and water extraction of 80 percent; taking roots, and preparing a root extract by adopting a water extraction step; preparing the dendrobium enzymatic hydrolysate by using cellulase and lactic acid bacteria. The method comprises the steps of taking ammonium ceric nitrate as an initiator, grafting polyethylene glycol methacrylate onto the surface of a nano cellulose crystal, and then complexing with alpha-cyclodextrin, a dendrobe stem and leaf extract, a dendrobe root extract, a dendrobe enzymolysis fermentation product and glycerol to form supermolecule hydrogel with oxidation resistance, so that the whole dendrobe is fully utilized, and resources are saved.
Description
Technical Field
The invention belongs to the technical field of antioxidant materials, and particularly relates to a preparation method, a product and application of a dendrobium extract-nano cellulose composite hydrogel.
Background
The hydrogel is a high water absorption and high water retention material and is widely used in various fields. For example, the compound is used as a drought resistant agent in arid regions, as a moisturizing agent such as a mask and an analgesic patch in cosmetics, and as a film humidity regulator in agriculture. As a water-absorbing and water-retaining material, hydrogel has different requirements for molecular weight, specific consumables and the like when being applied to different fields.
Currently, in the field of cosmetics, the raw materials for preparing hydrogel mainly include substances such as a colloidal substance, a plant extract, a gelling agent, glycerin and the like. The gel, glycerin and gelling agent are mainly used for forming the product into a hydrogel state, so that the product is convenient to wipe evenly, absorb water and preserve moisture, and the plant extract is mainly used for improving the skin care effect of the hydrogel by using the rich effective substances in the plant extract. For example, chinese patent CN104127605B discloses an aloe essential oil hydrogel acne-removing patch and a manufacturing method thereof, the patch is prepared from various plant extracts such as aloe, persimmon leaves, rhubarb, wild chrysanthemum flower and the like, and has the effects of high absorption rate, low allergy and acne removal.
The dendrobium contains various effective components such as dendrobine, flavone, amino acid, dendrobe polysaccharide and the like, can be used as one of preparation materials of hydrogel, and has good application prospect in the fields of skin care and the like. However, in the prior art, when the dendrobium hydrogel is prepared, the dendrobium polysaccharide extract is adopted, and the rest of dendrobium plants are discarded as waste materials, so that resources are wasted.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method, a product and application of dendrobium extract-nano cellulose composite hydrogel.
The invention aims to provide a preparation method of dendrobium extract-nano cellulose composite hydrogel,
step 1, preparing a dendrobe stem and leaf extract and a dendrobe root extract
Cleaning fresh herba Dendrobii, air drying, cutting from the root-stem junction, and respectively preserving root and stem-leaf;
adding 80% ethanol solution into stem and leaf part, extracting, filtering, collecting stem and leaf ethanol extract and stem and leaf ethanol extract precipitate respectively, adding distilled water into stem and leaf ethanol extract precipitate, extracting, filtering, and collecting stem and leaf water extract and stem and leaf water extract precipitate; combining the stem and leaf alcohol extract and the stem and leaf water extract, concentrating and drying to obtain the stem and leaf extract of the dendrobium;
taking roots, adding distilled water, leaching, filtering, and collecting root extract and root precipitate; concentrating the root extract, and drying to obtain root extract;
step 2, preparing the dendrobium enzymolysis fermentation product
Mixing the stem leaf water extract sediment and the root sediment, and crushing to obtain a sediment mixture; adding cellulase liquid into the precipitate mixture for enzymolysis, then inactivating enzymes, adding lactobacillus liquid, fermenting at 30 +/-1 ℃ for 36-48 h, filtering, collecting fermentation supernatant, volatilizing a dry solvent, then adding 2 times of purified water by mass, and mixing to obtain a dendrobe enzymolysis ferment;
wherein the proportion of the precipitation mixture, the cellulase solution and the lactobacillus solution is 5g: 1-5 g:100 mL;
step 3, preparation of hydrogel
The hydrogel is prepared from the following raw materials: the feed additive comprises a dendrobium stem and leaf extract, a dendrobium root extract, a dendrobium enzymolysis fermentation product, 1g/100mL of nano cellulose crystal liquid, alpha-cyclodextrin, polyethylene glycol methacrylate, ammonium ceric nitrate and glycerol.
Preferably, in the preparation method of the dendrobium extract-nanocellulose composite hydrogel, when the dendrobium stem and leaf extract is prepared, the proportion of the stem and leaf part, the 80% ethanol solution and the distilled water is 1g: 100-: 100-; (ii) a Each leaching time is 0.5-1.5 h.
Preferably, in the preparation method of the dendrobium extract-nano cellulose composite hydrogel, when the root extract is prepared, the proportion of the root to distilled water is 1g to 100 mL; the leaching time is 0.5-1 h.
Preferably, in the preparation method of the dendrobium extract-nano cellulose composite hydrogel, when the dendrobium enzymolysis fermentation product is prepared, the concentration of the cellulase liquid is 2g/L, and the enzymolysis condition is enzymolysis for 4 hours at 40 ℃; the enzyme inactivating condition is that the treatment is carried out for 1min at 95-100 ℃, and the lactobacillus liquid is added after natural cooling.
Preferably, in the preparation method of the dendrobium extract-nano cellulose composite hydrogel, the lactobacillus bacterial liquid is lactobacillus fermentum ATCC 11739 bacterial liquid, and the viable count in the bacterial liquid is more than or equal to 106cfu/mL。
Preferably, in the preparation method of the dendrobium extract-nano cellulose composite hydrogel, when the dendrobium enzymolysis fermentation product is prepared, the concentration of the cellulase liquid is 2 g/L.
Preferably, the preparation method of the dendrobium extract-nanocellulose composite hydrogel comprises the following steps: 5-15 parts of dendrobium stem and leaf extract, 5-15 parts of dendrobium root extract, 30-50 parts of dendrobium enzymolysis fermentation product, 150 parts of 1g/100mL nano-cellulose crystal liquid, 20-25 parts of alpha-cyclodextrin, 3 parts of polyethylene glycol methacrylate, 0.15-0.20 part of ammonium ceric nitrate and 10-20 parts of glycerol.
Preferably, the preparation method of the dendrobium extract-nanocellulose composite hydrogel comprises the following specific preparation methods:
mixing polyethylene glycol methacrylate with the nano cellulose crystal, adjusting the pH value to 1.8-2.0, stirring for 5-10min under the nitrogen atmosphere, adding ammonium ceric nitrate, continuously stirring and reacting for 24-30h under the nitrogen atmosphere, centrifuging at 10000-15000r/min, removing the supernatant, and collecting a hydrogel carrier;
adding 2 times of purified water by mass into a hydrogel carrier, stirring for 5-10min in a water bath at 55 ℃, then adding alpha-cyclodextrin and glycerol, continuing stirring for 5-10min in a water bath at 55 ℃, then adding a dendrobe stem leaf extract, a dendrobe root extract and a dendrobe enzymolysis fermentation product, stirring for 5-10min in a water bath at 55 ℃, and standing to obtain the dendrobe extract-nano cellulose composite hydrogel.
The invention also provides the dendrobe extract-nano cellulose composite hydrogel or dendrobe enzymolysis leavening prepared by the method.
The invention also provides application of the dendrobe enzymatic hydrolysate or dendrobe extract-nano cellulose composite hydrogel or dendrobe enzymatic hydrolysate in preparation of an antioxidant product.
Compared with the prior art, the preparation method of the dendrobium extract-nano cellulose composite hydrogel provided by the invention has the following beneficial effects:
the method comprises the steps of respectively treating roots and stem leaves of the whole plant of the dendrobium, preparing a dendrobium stem and leaf extract and a dendrobium root extract, and then preparing a dendrobium enzymolysis zymolyte by using cellulase and lactic acid bacteria. Ammonium ceric nitrate (CAN) is used as an initiator, polyethylene glycol methacrylate is grafted to the surface of the nano-cellulose crystal, and then is complexed with alpha-cyclodextrin, dendrobe stem leaf extract, dendrobe root extract, dendrobe enzymolysis fermentation product and glycerol to form supermolecule hydrogel with oxidation resistance, dendrobe whole grass is fully utilized, and resources are saved.
In the preparation method provided by the invention, the stem and leaf parts contain more chlorophyll, pigment and other substances, so that an alcohol-soluble substance such as the pigment is extracted by using an alcohol-extracting and distilled water-extracting two-step method, namely, an 80% alcohol solution, and then a water-soluble substance is extracted by using distilled water, so that the extraction efficiency is high. The cellulose is degraded into small molecules by the action of the cellulase, so that the lactobacillus can be conveniently utilized. After the lactobacillus is fermented, the oxidation resistance of the product can be improved, and the prepared hydrogel product can be used in the fields of skin care and the like.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention to practice, the present invention will be further described with reference to the following specific examples.
In the present invention, all reagents are commercially available unless otherwise specified.
In the invention, the room temperature refers to the temperature of 20-40 ℃, and if the temperature is lower than 20 ℃, a water bath mode can be adopted.
The lactobacillus used in the invention is Lactobacillus fermentum ATCC 11739 (Sichuan Rui Nuo Sa Biotech Co., Ltd., viable count of lactobacillus solution is not less than 106cfu/mL). The nano-cellulose crystal liquid is prepared from nano-cellulose crystal (CNC) which is obtained by acid hydrolysis of natural cellulose, has a surface rich in hydroxyl, and is purchased from assist in new material science and technology (Shanghai) Co., Ltd, and has the appearance: a white gel; solid content: 6 percent; density: 1.05g/cm3(ii) a Average particle size: the width is 4-5nm, and the length is 50-500 nm; crystallinity (XRD): 93 percent. The polyethylene glycol methacrylate used had an average molecular weight Mw of 500 (Sigma).
In the preparation process of the stem leaf extract and the root extract of the dendrobium, roots and stem leaves need to be cut into small sections of 1-2cm, and then extraction operation is carried out.
In the following examples and comparative examples of the present invention, each part by weight corresponds to 1g by mass.
In the invention, the antioxidant activity of' Wanghua.3 medicinal dendrobe polysaccharides is referred to for comparative research [ J ]. the university of south China, proceedings: natural science edition, 2015 (47): 65-70 "method for determining DPPH radical clearance and superoxide anion radical clearance.
Example 1
A preparation method of dendrobium extract-nanocellulose composite hydrogel comprises the following steps:
step 1, preparing a dendrobe stem and leaf extract and a dendrobe root extract
Cleaning fresh whole herba Dendrobii with tap water, naturally drying, cutting from the root-stem junction (the position where the root and beard begin to grow), and respectively preserving the root and stem-leaf parts;
taking stem and leaf parts, adding 80% ethanol solution, standing and extracting at room temperature for 0.5h, filtering with two layers of gauze, respectively collecting stem and leaf ethanol extract and stem and leaf ethanol extract precipitate, adding distilled water into stem and leaf ethanol extract precipitate, standing and extracting at room temperature for 1h, filtering with gauze, and collecting stem and leaf water extract and stem and leaf water extract precipitate; mixing the alcoholic extractive solution and water extract, concentrating under reduced pressure, and freeze drying to obtain stem and leaf extract of herba Dendrobii; the ratio of the stem and leaf part, the 80% ethanol solution and the distilled water is 1g:100mL:100 mL;
taking roots, adding distilled water, wherein the ratio of the roots to the distilled water is 1g to 100 mL; standing at room temperature, leaching for 0.5h, filtering with two layers of gauze, and collecting root extractive solution and root precipitate; concentrating the root extractive solution under reduced pressure, and freeze drying to obtain root extract;
step 2, preparing the dendrobium enzymolysis fermentation product
Mixing the stem leaf water extraction sediment and the root sediment, grinding the mixture to crush the sediment into paste (the ground state is semisolid paste due to high water content of the stem leaf water extraction sediment and the root sediment), and obtaining a sediment mixture; adding 2g/L cellulase solution into the precipitate mixture, performing enzymolysis for 4h at 40 ℃, performing enzyme deactivation treatment for 1min at 95 ℃, naturally cooling, adding lactobacillus bacteria solution, fermenting for 36h at 30 +/-1 ℃, filtering, collecting fermentation supernatant, volatilizing a dry solvent, adding purified water with the mass 2 times that of the precipitate, and performing homogeneous mixing to obtain a dendrobe enzymolysis zymolyte;
wherein the proportion of the precipitation mixture, 2g/L cellulase liquid and lactobacillus liquid is 5g:1g:100 mL;
step 3, preparation of hydrogel
The hydrogel is prepared from the following raw materials in parts by weight: 5 parts of dendrobium stem and leaf extract, 5 parts of dendrobium root extract, 30 parts of dendrobium enzymolysis leavening, 150 parts of 1g/100mL nano cellulose crystal liquid, 20 parts of alpha-cyclodextrin, 3 parts of polyethylene glycol methacrylate, 0.15 part of ammonium ceric nitrate and 10 parts of glycerol. Weighing the raw materials in parts by weight.
Adding polyethylene glycol methacrylate and a nano cellulose crystal into a 500mL reaction bottle, adjusting the pH value to 1.8 by using nitric acid, stirring for 5min under a nitrogen atmosphere, then adding ammonium ceric nitrate, continuously stirring and reacting for 24h under the nitrogen atmosphere, centrifuging for 20min at 15000r/min, and removing a supernatant to obtain a hydrogel carrier;
adding 2 times of purified water by mass into a hydrogel carrier, stirring in a water bath at 55 ℃ for 5min, then adding alpha-cyclodextrin and glycerol, continuing to stir in the water bath at 55 ℃ for 5min, then adding the dendrobium stem and leaf extract, the dendrobium root extract and the dendrobium enzymolysis leavening, stirring in the water bath at 55 ℃ for 10min, and standing for 10min to obtain the dendrobium extract-nano cellulose composite hydrogel.
The dendrobe extract-nano cellulose composite hydrogel is prepared into 2g/L mixed solution, and then the free radical clearance rate is measured, wherein the superoxide anion free radical clearance rate is 23.8%, and the DPPH free radical clearance rate is 15.4%.
Example 2
A preparation method of dendrobium extract-nanocellulose composite hydrogel comprises the following steps:
step 1, preparing a dendrobe stem and leaf extract and a dendrobe root extract
Cleaning fresh whole herba Dendrobii with tap water, naturally drying, cutting from the root-stem junction (the position where the root and beard begin to grow), and respectively preserving the root and stem-leaf parts;
taking stem and leaf parts, adding 80% ethanol solution, standing and extracting at room temperature for 1h, filtering with two layers of gauze, respectively collecting stem and leaf ethanol extract and stem and leaf ethanol extract precipitate, adding distilled water into stem and leaf ethanol extract precipitate, standing and extracting at room temperature for 1.5h, filtering with two layers of gauze, and collecting stem and leaf water extract and stem and leaf water extract precipitate; mixing the alcoholic extractive solution and water extract, concentrating under reduced pressure, and freeze drying to obtain stem and leaf extract of herba Dendrobii; the ratio of the stem and leaf part, the 80% ethanol solution and the distilled water is 1g:150mL:100 mL;
taking roots, adding distilled water, wherein the ratio of the roots to the distilled water is 1g to 100 mL; standing at room temperature, leaching for 1h, filtering with two layers of gauze, and collecting root extractive solution and root precipitate; concentrating the root extractive solution under reduced pressure, and freeze drying to obtain root extract;
step 2, preparing the dendrobium enzymolysis fermentation product
Mixing the stem leaf water extraction precipitate and the root precipitate, grinding the mixture to crush the precipitate into paste, and obtaining a precipitate mixture; adding 2g/L cellulase solution into the precipitate mixture, performing enzymolysis for 4h at 40 ℃, performing enzyme deactivation treatment for 1min at 100 ℃, naturally cooling, adding lactobacillus liquid, fermenting for 48h at 30 +/-1 ℃, filtering, collecting fermentation supernatant, volatilizing a dry solvent, adding purified water with the mass 2 times that of the precipitate, and performing homogeneous mixing to obtain a dendrobe enzymolysis zymolyte;
wherein the proportion of the precipitation mixture, 2g/L cellulase liquid and lactobacillus liquid is 5g:5g:100 mL;
step 3, preparation of hydrogel
The hydrogel is prepared from the following raw materials in parts by weight: 15 parts of dendrobium stem and leaf extract, 15 parts of dendrobium root extract, 50 parts of dendrobium enzymolysis leavening, 150 parts of 1g/100mL nano-cellulose crystal liquid, 25 parts of alpha-cyclodextrin, 3 parts of polyethylene glycol methacrylate, 0.2 part of ammonium ceric nitrate and 20 parts of glycerol. Weighing the raw materials in parts by weight.
Adding polyethylene glycol methacrylate and a nano cellulose crystal into a 500mL reaction bottle, adjusting the pH value to 2 by using nitric acid, stirring for 10min under a nitrogen atmosphere, then adding cerium ammonium nitrate, continuously stirring and reacting for 30h under the nitrogen atmosphere, centrifuging for 20min at 15000r/min, and removing a supernatant to obtain a hydrogel carrier;
adding 2 times of purified water by mass into a hydrogel carrier, stirring in a water bath at 55 ℃ for 10min, then adding alpha-cyclodextrin and glycerol, continuing stirring in a water bath at 55 ℃ for 10min, then adding the dendrobium stem and leaf extract, the dendrobium root extract and the dendrobium enzymolysis leavening, stirring in a water bath at 55 ℃ for 5min, and standing for 15min to obtain the dendrobium extract-nano cellulose composite hydrogel.
The dendrobe extract-nano cellulose composite hydrogel is prepared into 2g/L mixed solution, and then the free radical clearance rate is measured, wherein the superoxide anion free radical clearance rate is 21.7%, and the DPPH free radical clearance rate is 16.9%.
Example 3
A preparation method of dendrobium extract-nanocellulose composite hydrogel comprises the following steps:
step 1, preparing a dendrobe stem and leaf extract and a dendrobe root extract
Cleaning fresh whole herba Dendrobii with tap water, naturally drying, cutting from the root-stem junction (the position where the root and beard begin to grow), and respectively preserving the root and stem-leaf parts;
taking stem and leaf parts, adding 80% ethanol solution, standing and extracting at room temperature for 0.5h, filtering with two layers of gauze, respectively collecting stem and leaf ethanol extract and stem and leaf ethanol extract precipitate, adding distilled water into stem and leaf ethanol extract precipitate, standing and extracting at room temperature for 1h, filtering with two layers of gauze, and collecting stem and leaf water extract and stem and leaf water extract precipitate; mixing the alcoholic extractive solution and water extract, concentrating under reduced pressure, and freeze drying to obtain stem and leaf extract of herba Dendrobii; the ratio of the stem and leaf part, the 80% ethanol solution and the distilled water is 1g:125mL:100 mL;
taking roots, adding distilled water, wherein the ratio of the roots to the distilled water is 1g to 100 mL; standing at room temperature, leaching for 0.5h, filtering with two layers of gauze, and collecting root extractive solution and root precipitate; concentrating the root extractive solution under reduced pressure, and freeze drying to obtain root extract;
step 2, preparing the dendrobium enzymolysis fermentation product
Mixing the stem leaf water extraction precipitate and the root precipitate, grinding the mixture to crush the precipitate into paste, and obtaining a precipitate mixture; adding 2g/L cellulase solution into the precipitate mixture, performing enzymolysis for 4h at 40 ℃, performing enzyme deactivation treatment for 1min at 95 ℃, naturally cooling, adding lactobacillus bacteria solution, fermenting for 36h at 30 +/-1 ℃, filtering, collecting fermentation supernatant, volatilizing a dry solvent, adding purified water with the mass 2 times that of the precipitate, and performing homogeneous mixing to obtain a dendrobe enzymolysis zymolyte;
wherein the proportion of the precipitation mixture, 2g/L cellulase liquid and lactobacillus liquid is 5g:3g:100 mL;
step 3, preparation of hydrogel
The hydrogel is prepared from the following raw materials in parts by weight: 10 parts of dendrobium stem and leaf extract, 10 parts of dendrobium root extract, 40 parts of dendrobium enzymolysis leavening, 150 parts of 1g/100mL nano-cellulose crystal liquid, 20 parts of alpha-cyclodextrin, 3 parts of polyethylene glycol methacrylate, 0.15 part of ammonium ceric nitrate and 10 parts of glycerol. Weighing the raw materials in parts by weight.
Adding polyethylene glycol methacrylate and a nano cellulose crystal into a 500mL reaction bottle, adjusting the pH value to 1.8 by using nitric acid, stirring for 5min under a nitrogen atmosphere, then adding ammonium ceric nitrate, continuously stirring and reacting for 24h under the nitrogen atmosphere, centrifuging for 20min at 15000r/min, and removing a supernatant to obtain a hydrogel carrier;
adding 2 times of purified water by mass into a hydrogel carrier, stirring in a water bath at 55 ℃ for 5min, then adding alpha-cyclodextrin and glycerol, continuing to stir in the water bath at 55 ℃ for 5min, then adding the dendrobium stem and leaf extract, the dendrobium root extract and the dendrobium enzymolysis leavening, stirring in the water bath at 55 ℃ for 10min, and standing for 10min to obtain the dendrobium extract-nano cellulose composite hydrogel.
The dendrobe extract-nano cellulose composite hydrogel is prepared into a mixed solution of 2g/L, and then the free radical clearance rate is measured, wherein the superoxide anion free radical clearance rate is 19.4%, and the DPPH free radical clearance rate is 15.7%.
According to the invention, the roots and the stem and leaf parts of the whole herb of dendrobium are respectively treated to prepare the stem and leaf extract and the root extract of dendrobium, then the enzymolysis fermentation product of dendrobium is prepared by using cellulase and lactic acid bacteria, the whole herb of dendrobium is fully utilized, and the prepared stem and leaf extract, root extract and enzymolysis fermentation product of dendrobium have antioxidant effects. Meanwhile, the influence of different extraction methods on the oxidation resistance of the stem and leaf extract and the enzymolysis fermentation product of the dendrobium is also explored, and relevant comparative experiments are as follows:
comparative example 1
The method for investigating the influence of different extraction modes on the oxidation resistance of the dendrobe stem leaf extract comprises the following steps: cleaning fresh whole herba Dendrobii with tap water, naturally drying, cutting from the root-stem junction (the position where the root and beard begin to grow), and respectively preserving the root and stem-leaf parts; taking stem and leaf parts, adding 80% ethanol solution by volume fraction, reflux extracting in 55 deg.C water bath for 1.5 hr, filtering with two layers of gauze, respectively collecting stem and leaf ethanol extract and stem and leaf ethanol extract precipitate, concentrating the stem and leaf ethanol extract under reduced pressure, and freeze drying to obtain stem and leaf extract of herba Dendrobii; the ratio of the stem and leaf parts to the 80% ethanol solution was 1g:100 mL.
The stem and leaf extract of dendrobium nobile in the comparative example 1 is prepared into 2g/L mixed solution, and then the free radical clearance is measured, wherein the free radical clearance of superoxide anion is 38.7 percent, and the free radical clearance of DPPH is 27.5 percent.
The stem and leaf extract of dendrobium nobile is prepared according to the method of the embodiment 1, mixed liquor of 2g/L is prepared, and then the free radical clearance is measured, wherein the free radical clearance of superoxide anions is 71.4 percent, and the free radical clearance of DPPH is 59.6 percent.
Comparative example 2
Investigating the influence of different extraction modes on the oxidation resistance of the dendrobe enzymolysis fermentation product, and the specific method comprises the following steps:
respectively preparing stem and leaf water extraction precipitates and mixing the root precipitates according to the method of example 1, grinding the precipitates into paste, and obtaining a precipitate mixture; adding lactobacillus bacteria liquid into the precipitate mixture, wherein the proportion of the precipitate mixture to the lactobacillus bacteria liquid is 5g:100mL, fermenting for 36h at 30 +/-1 ℃, filtering by two layers of gauze, collecting fermentation supernatant, volatilizing the solvent, adding purified water with the mass 2 times that of the precipitate, and homogenizing and mixing to obtain the dendrobium enzymatic hydrolysate.
Preparing the dendrobium enzymatic hydrolysate of the comparative example 1 into 2g/L mixed solution, and then measuring the free radical clearance rate, wherein the superoxide anion free radical clearance rate is 23.1%, and the DPPH free radical clearance rate is 18.2%.
The dendrobe enzymolysis fermentation product is prepared according to the method of example 1, mixed liquor of 2g/L is prepared, and then the free radical clearance rate is measured, wherein the superoxide anion free radical clearance rate is 56.4%, and the DPPH free radical clearance rate is 37.0%.
The comparative example 1 lacks the enzymolysis step of the cellulase, is not beneficial to the hydrolysis of the cellulose in the stem and the root of the dendrobium stem, and causes difficulty in the utilization of lactic acid bacteria, so the fermentation efficiency is low, and the prepared dendrobium enzymolysis leavening has low oxidation resistance.
Comparative example 3
Investigating the influence of different extraction modes on the oxidation resistance of the dendrobe enzymolysis fermentation product, and the specific method comprises the following steps:
the aqueous extract precipitates of the stems and leaves and the precipitates of the roots, which were prepared separately according to the method of example 1, were mixed and ground to pulverize the precipitates into a paste, thereby obtaining a precipitate mixture. Preparing the dendrobium enzymolysis fermentation product of the comparative example 1 into 2g/L mixed solution, and then measuring the free radical clearance rate, wherein the superoxide anion free radical clearance rate is 15.4%, and the DPPH free radical clearance rate is 8.7%. Comparative document 3 has no treatment of the extracted precipitate, and thus the antioxidant ability is the lowest.
It should be noted that, when the present invention relates to a numerical range, it should be understood that two endpoints of each numerical range and any value between the two endpoints can be selected, and since the steps and methods adopted are the same as those in the embodiment, in order to prevent redundancy, the present invention describes a preferred embodiment. While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (9)
1. A preparation method of dendrobium extract-nano cellulose composite hydrogel is characterized by comprising the following steps:
step 1, preparing a dendrobe stem and leaf extract and a dendrobe root extract
Cleaning fresh herba Dendrobii, air drying, cutting from the root-stem junction, and respectively preserving root and stem-leaf;
taking stem and leaf parts, adding ethanol solution with volume fraction of 80%, leaching, filtering, respectively collecting stem and leaf ethanol extract and stem and leaf ethanol extract precipitate, adding distilled water into stem and leaf ethanol extract precipitate, leaching, filtering, and collecting stem and leaf water extract and stem and leaf water extract precipitate; combining the stem and leaf alcohol extract and the stem and leaf water extract, concentrating and drying to obtain the stem and leaf extract of the dendrobium;
taking roots, adding distilled water, leaching, filtering, and collecting root extract and root precipitate; concentrating the root extract, and drying to obtain root extract;
step 2, preparing the dendrobium enzymolysis fermentation product
Mixing the stem leaf water extract sediment and the root sediment, and crushing to obtain a sediment mixture; adding cellulase liquid into the precipitate mixture for enzymolysis, then inactivating enzymes, adding lactobacillus liquid, fermenting at 30 +/-1 ℃ for 36-48 h, filtering, collecting fermentation supernatant, volatilizing a dry solvent, then adding 2 times of purified water by mass, and mixing to obtain a dendrobe enzymolysis ferment;
wherein the proportion of the precipitation mixture, the cellulase solution and the lactobacillus solution is 5g: 1-5 g:100 mL;
step 3, preparation of hydrogel
The hydrogel is prepared from the following raw materials: the feed additive comprises a dendrobium stem and leaf extract, a dendrobium root extract, a dendrobium enzymolysis fermentation product, 1g/100mL of nano cellulose crystal liquid, alpha-cyclodextrin, polyethylene glycol methacrylate, ammonium ceric nitrate and glycerol.
2. The method for preparing the dendrobium extract-nanocellulose composite hydrogel as claimed in claim 1, wherein when the dendrobium stem and leaf extract is prepared, the ratio of the stem and leaf part, the 80% ethanol solution and the distilled water is 1g: 100-: 100-; each leaching time is 0.5-1.5 h.
3. The method for preparing the dendrobium extract-nanocellulose composite hydrogel according to claim 1, wherein when preparing the root extract, the ratio of the root to distilled water is 1g:100 mL; the leaching time is 0.5-1 h.
4. The preparation method of the dendrobe extract-nanocellulose composite hydrogel according to claim 1, wherein when preparing the dendrobe enzymatic hydrolysate, the concentration of cellulase liquid is 2g/L, and the enzymatic hydrolysis condition is 40 ℃ for 4 h; the enzyme inactivating condition is that the treatment is carried out for 1min at 95-100 ℃, and the lactobacillus liquid is added after natural cooling.
5. The method for preparing the dendrobium extract-nanocellulose composite hydrogel according to claim 4, wherein the lactobacillus bacterial liquid is lactobacillus fermentum ATCC 11739 bacterial liquid, and the number of viable bacteria in the bacterial liquid is more than or equal to 106cfu/mL。
6. The preparation method of the dendrobium extract-nanocellulose composite hydrogel according to claim 1, wherein the hydrogel is prepared from the following raw materials in parts by weight: 5-15 parts of dendrobium stem and leaf extract, 5-15 parts of dendrobium root extract, 30-50 parts of dendrobium enzymolysis fermentation product, 150 parts of 1g/100mL nano-cellulose crystal liquid, 20-25 parts of alpha-cyclodextrin, 3 parts of polyethylene glycol methacrylate, 0.15-0.20 part of ammonium ceric nitrate and 10-20 parts of glycerol.
7. The preparation method of the dendrobium extract-nanocellulose composite hydrogel according to claim 6, wherein the specific preparation method of the hydrogel is as follows:
mixing polyethylene glycol methacrylate with the nano cellulose crystal, adjusting the pH value to 1.8-2.0, stirring for 5-10min under the nitrogen atmosphere, adding ammonium ceric nitrate, continuously stirring and reacting for 24-30h under the nitrogen atmosphere, centrifuging at 10000-15000r/min, removing the supernatant, and collecting a hydrogel carrier;
adding 2 times of purified water by mass into a hydrogel carrier, stirring for 5-10min in a water bath at 55 ℃, then adding alpha-cyclodextrin and glycerol, continuing stirring for 5-10min in a water bath at 55 ℃, then adding a dendrobe stem leaf extract, a dendrobe root extract and a dendrobe enzymolysis fermentation product, stirring for 5-10min in a water bath at 55 ℃, and standing to obtain the dendrobe extract-nano cellulose composite hydrogel.
8. The dendrobe extract-nanocellulose composite hydrogel or dendrobe enzymatic hydrolysate prepared by the method according to any one of claims 1 to 7.
9. The use of the enzymatic hydrolysate of dendrobium nobile as claimed in claim 8 or the composite hydrogel of dendrobium nobile extract and nanocellulose or the enzymatic hydrolysate of dendrobium nobile in the preparation of antioxidant products.
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