CN115232516B - Anti-adhesion coating with camellia saponin as main component, preparation method thereof and application thereof in inhibiting bacillus cereus - Google Patents

Anti-adhesion coating with camellia saponin as main component, preparation method thereof and application thereof in inhibiting bacillus cereus Download PDF

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CN115232516B
CN115232516B CN202210736610.2A CN202210736610A CN115232516B CN 115232516 B CN115232516 B CN 115232516B CN 202210736610 A CN202210736610 A CN 202210736610A CN 115232516 B CN115232516 B CN 115232516B
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tea
saponin
oil
ethanol
parts
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CN115232516A (en
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高一丹
马英姿
刘思思
涂佳
肖静晶
肖志红
李昌珠
吉悦娜
李力
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Central South University of Forestry and Technology
Hunan Academy of Forestry
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Hunan Academy of Forestry
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Abstract

The invention discloses an anti-adhesion coating taking tea-oil saponin as a main component, a preparation method thereof and application thereof in inhibiting bacillus cereus, and relates to the technical field of bacteriostat, wherein the anti-adhesion coating taking tea-oil saponin as the main component comprises 55-80 parts by weight of tea-oil saponin, 15-30 parts by weight of polypropylene, 2-3 parts by weight of ginkgolic acid, 1-2 parts by weight of rheum officinale extract and 0.5-1 part by weight of ootheca mantis lipid extract; a method of preparing an anti-tack coating comprising the steps of: s1: extracting oil tea saponin; s2: extracting ginkgolic acid; s3: preparing rheum officinale extract; s4: preparing an anti-adhesive coating with tea saponin as a main component: the anti-adhesion coating taking the tea saponin as a main component has the antibacterial effect of destroying the adhesion of bacillus cereus and destroying the structure of a biological film so as to play a role in inhibiting the bacillus cereus and reduce the drug resistance of bacteria; the oil tea saponin is extracted from byproduct oil tea cakes after oil tea oil extraction, and the resource is reused and the cost is low.

Description

Anti-adhesion coating with camellia saponin as main component, preparation method thereof and application thereof in inhibiting bacillus cereus
Technical Field
The invention relates to the technical field of bacteriostats, in particular to an anti-adhesion coating taking tea-oil camellia saponin as a main component, a preparation method thereof and application thereof in inhibiting bacillus cereus.
Background
The bacillus cereus can cause food poisoning in foods such as rice and flour products, bean products, dairy products, bulk cooked meat products and the like, antibiotics are adopted to inhibit the bacillus cereus at present, but the excessive amount of the antibiotics and the drug residues of livestock products not only affect environmental pollution, but also cause the enhancement of drug resistance of more and more bacteria to the antibiotics; the tea saponin is pentacyclic triterpene compound containing structural sugar and structural acid extracted from tea cake after oil extraction of tea seed, and has antibacterial, antiinflammatory, antihypertensive, antitumor, insecticidal and anthelmintic effects; the anti-adhesive coating taking the tea saponin as a main component is used for destroying the adhesion of bacillus cereus and destroying the structure of a biological envelope so as to inhibit the bacillus cereus; the development pollution of the oil tea saponin is small, and the oil tea saponin is extracted by using the oil tea seed cake, so that the raw materials are abundant and cheap, the cost is low, and the harm is small.
Disclosure of Invention
In view of the above, the present invention aims at overcoming the defects of the prior art, and the main purpose of the present invention is to provide an anti-adhesion coating using tea saponin as a main component, a preparation method thereof and an application thereof in inhibiting bacillus cereus, wherein the anti-adhesion coating using tea saponin as a main component is prepared by adopting tea saponin, polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantis lipid extract, and the anti-adhesion coating using tea saponin as a main component damages a biological film structure so as to play a role in inhibiting bacillus cereus, and reduce bacterial drug resistance.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
an anti-adhesive coating taking tea saponin as a main component comprises, by weight, 55-80 parts of tea saponin, 15-30 parts of polypropylene, 2-3 parts of ginkgolic acid, 1-2 parts of rheum officinale extract and 0.5-1 part of ootheca mantidis lipid extract; the oil tea saponin is extracted from a byproduct oil tea cake obtained after oil tea seed oil extraction, and the process for extracting the oil tea saponin from the oil tea cake comprises ethanol extraction and polyamide chromatographic column extraction.
As a preferred embodiment: 75 parts of tea-oil camellia saponin.
As a preferred embodiment: the total weight percentage of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5%.
The preparation method of the anti-adhesion coating taking the tea-oil camellia saponin as the main component comprises the following steps:
s1: extracting tea-oil camellia saponin: pulverizing oil tea cake, extracting with 80% ethanol, and concentrating the extractive solution to obtain concentrated solution; gradient eluting the concentrated solution by adopting a polyamide chromatographic column, and respectively collecting and measuring the eluted liquid to obtain the sasanqua saponin;
s2: extracting ginkgolic acid: crushing bitter gingko, adding water for dissolution, adopting a macroporous adsorption resin column to perform gradient elution on the dissolution liquid by using 30% and 78% ethanol, recovering the eluent, drying and concentrating, then adopting a silica gel column for elution, sequentially performing gradient elution by using petroleum ether-ethyl acetate with the volume ratio of 45:1, 35:1, 25:1, 15:1 and 5:1, respectively collecting the eluted liquid, and measuring to obtain bitter gingko phenolic acid;
s3: preparing rheum officinale extract: pulverizing radix et rhizoma Rhei, extracting with water under reflux, concentrating the extractive solution to obtain concentrated solution, adding 60% -78% ethanol, and extracting under reflux to obtain radix et rhizoma Rhei extract;
s4: preparing an anti-adhesive coating with tea saponin as a main component: according to the weight portions, 55 to 80 portions of tea saponin, 15 to 30 portions of polypropylene, 2 to 3 portions of ginkgolic acid, 1 to 2 portions of rheum officinale extract and 0.5 to 1 portion of ootheca mantidis lipid extract are evenly mixed.
As a preferred embodiment: the eluent adopted in the S1 is water, 30% ethanol, 50% ethanol, 70% ethanol, 90% ethanol and 95% ethanol.
The application of the anti-adhesion coating taking the tea saponin as the main component in inhibiting bacillus cereus is that the anti-adhesion coating taking the tea saponin as the main component is used for inhibiting bacillus cereus in food.
As a preferred embodiment: the anti-adhesion coating taking the camellia saponin as a main component is used for destroying bacillus cereus to adhere to the surface of a carrier, destroying a biological film structure and further inhibiting the bacillus cereus.
As a preferred embodiment: the anti-sticking coating taking the tea-oil camellia saponin as a main component is smeared on a pipeline or a corner position of food processing equipment.
Compared with the prior art, the invention has obvious advantages and beneficial effects, in particular, the technical proposal shows that the invention adopts the tea saponin, the polypropylene, the ginkgolic acid, the rheum officinale extract and the ootheca mantidis lipid extract to prepare the anti-adhesion coating taking the tea saponin as the main component, and the anti-adhesion coating taking the tea saponin as the main component has the antibacterial effect of destroying the adhesion of bacillus cereus, destroying the biological membrane structure, further playing the inhibition role on the bacillus cereus and reducing the drug resistance of bacteria; the anti-sticking coating has the main components of tea saponin, the tea saponin is extracted from a byproduct tea cake after the tea oil is extracted, the resource is reused, and the cost is low; the tea saponin is a plant extract, so that the influence on the environment caused by bacteriostasis by adopting antibiotics is avoided, and the tea saponin is safe, environment-friendly and low in toxicity.
In order to more clearly illustrate the structural features and efficacy of the present invention, a detailed description thereof will be given below with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a graph showing the bacteriostatic effect of the anti-sticking coatings prepared in examples 1-6 of the present invention;
FIG. 2 shows the anti-adhesive coating of the present invention at 1X 10 8 Inhibition biofilm effect profile at cfu/mL concentration;
FIG. 3 shows the anti-adhesive coating of the present invention at 1X 10 6 Graph of biofilm inhibition effect at cfu/mL concentration.
Detailed Description
An anti-adhesive coating taking tea saponin as a main component comprises, by weight, 55-80 parts of tea saponin, 15-30 parts of polypropylene, 2-3 parts of ginkgolic acid, 1-2 parts of rheum officinale extract and 0.5-1 part of ootheca mantidis lipid extract; the total weight percentage of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 percent; the oil tea saponin is extracted from byproduct oil tea cakes obtained after oil tea seed oil extraction; the process for extracting the tea-oil saponin from the tea-oil cake comprises ethanol extraction and polyamide chromatographic column extraction.
The preparation method of the anti-sticking coating with the tea saponin as the main component comprises the following steps:
s1: extracting tea-oil camellia saponin: pulverizing oil tea cake, extracting with 80% ethanol, and concentrating the extractive solution to obtain concentrated solution; gradient eluting the concentrated solution by adopting a polyamide chromatographic column, and respectively collecting and measuring the eluted liquid to obtain the sasanqua saponin; the eluent is water, 30% ethanol, 50% ethanol, 70% ethanol, 90% ethanol and 95% ethanol.
S2: extracting ginkgolic acid: crushing bitter gingko, adding water for dissolution, adopting a macroporous adsorption resin column to perform gradient elution on the dissolution liquid by using 30% and 78% ethanol, recovering the eluent, drying and concentrating, then adopting a silica gel column for elution, sequentially performing gradient elution by using petroleum ether-ethyl acetate with the volume ratio of 45:1, 35:1, 25:1, 15:1 and 5:1, respectively collecting the eluted liquid, and measuring to obtain bitter gingko phenolic acid;
s3: preparing rheum officinale extract: pulverizing radix et rhizoma Rhei, extracting with water under reflux, concentrating the extractive solution to obtain concentrated solution, adding 60% -78% ethanol, and extracting under reflux to obtain radix et rhizoma Rhei extract;
s4: preparing an anti-adhesive coating with tea saponin as a main component: according to the weight portions, 55 to 80 portions of tea saponin, 15 to 30 portions of polypropylene, 2 to 3 portions of ginkgolic acid, 1 to 2 portions of rheum officinale extract and 0.5 to 1 portion of ootheca mantidis lipid extract are evenly mixed.
The anti-adhesion coating with the camellia saponin as the main component is used for inhibiting bacillus cereus in food; the anti-adhesion coating taking the camellia saponin as a main component is used for destroying bacillus cereus to adhere to the surface of a carrier, destroying a biological film structure and further inhibiting the bacillus cereus; the anti-sticking coating with tea saponin as main component is smeared on the pipeline or corner position of food processing equipment.
Example 1
An anti-adhesive coating taking tea saponin as a main component comprises 55 parts by weight of tea saponin, 40 parts by weight of polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
The preparation method of the anti-sticking coating with the tea saponin as the main component comprises the following steps:
s1: extracting tea-oil camellia saponin: pulverizing oil tea cake, extracting with 80% ethanol, and concentrating the extractive solution to obtain concentrated solution; gradient eluting the concentrated solution by adopting a polyamide chromatographic column, and respectively collecting and measuring the eluted liquid to obtain the sasanqua saponin; the eluent used was water, 30% ethanol, 50% ethanol, 70% ethanol, 90% ethanol and 95% ethanol.
S2: extracting ginkgolic acid: crushing bitter gingko, adding water for dissolution, adopting a macroporous adsorption resin column to perform gradient elution on the dissolution liquid by using 30% and 78% ethanol, recovering the eluent, drying and concentrating, then adopting a silica gel column for elution, sequentially performing gradient elution by using petroleum ether-ethyl acetate with the volume ratio of 45:1, 35:1, 25:1, 15:1 and 5:1, respectively collecting the eluted liquid, and measuring to obtain bitter gingko phenolic acid;
s3: preparing rheum officinale extract: pulverizing radix et rhizoma Rhei, extracting with water under reflux, concentrating the extractive solution to obtain concentrated solution, adding 78% ethanol, and extracting under reflux to obtain radix et rhizoma Rhei extract;
s4: preparing an anti-adhesive coating with tea saponin as a main component: mixing oil tea saponin 55 parts, polypropylene 40 parts, ginkgolic acid, rheum officinale extract and ootheca Mantidis lipid extract uniformly in parts by weight; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
Example 2
An anti-adhesive coating taking tea saponin as a main component comprises 60 parts by weight of tea saponin, 35 parts by weight of polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
The preparation method of the anti-sticking coating with the tea saponin as the main component comprises the following steps:
s1: extracting tea-oil camellia saponin: pulverizing oil tea cake, extracting with 80% ethanol, and concentrating the extractive solution to obtain concentrated solution; gradient eluting the concentrated solution by adopting a polyamide chromatographic column, and respectively collecting and measuring the eluted liquid to obtain the sasanqua saponin; the eluent used was water, 30% ethanol, 50% ethanol, 70% ethanol, 90% ethanol and 95% ethanol.
S2: extracting ginkgolic acid: crushing bitter gingko, adding water for dissolution, adopting a macroporous adsorption resin column to perform gradient elution on the dissolution liquid by using 30% and 78% ethanol, recovering the eluent, drying and concentrating, then adopting a silica gel column for elution, sequentially performing gradient elution by using petroleum ether-ethyl acetate with the volume ratio of 45:1, 35:1, 25:1, 15:1 and 5:1, respectively collecting the eluted liquid, and measuring to obtain bitter gingko phenolic acid;
s3: preparing rheum officinale extract: pulverizing radix et rhizoma Rhei, extracting with water under reflux, concentrating the extractive solution to obtain concentrated solution, adding 78% ethanol, and extracting under reflux to obtain radix et rhizoma Rhei extract;
s4: preparing an anti-adhesive coating with tea saponin as a main component: mixing 60 parts of tea saponin, 35 parts of polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract uniformly in parts by weight; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
Example 3
An anti-adhesive coating taking tea saponin as a main component comprises 65 parts by weight of tea saponin, 30 parts by weight of polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
The preparation method of the anti-sticking coating with the tea saponin as the main component comprises the following steps:
s1: extracting tea-oil camellia saponin: pulverizing oil tea cake, extracting with 80% ethanol, and concentrating the extractive solution to obtain concentrated solution; gradient eluting the concentrated solution by adopting a polyamide chromatographic column, and respectively collecting and measuring the eluted liquid to obtain the sasanqua saponin; the eluent used was water, 30% ethanol, 50% ethanol, 70% ethanol, 90% ethanol and 95% ethanol.
S2: extracting ginkgolic acid: crushing bitter gingko, adding water for dissolution, adopting a macroporous adsorption resin column to perform gradient elution on the dissolution liquid by using 30% and 78% ethanol, recovering the eluent, drying and concentrating, then adopting a silica gel column for elution, sequentially performing gradient elution by using petroleum ether-ethyl acetate with the volume ratio of 45:1, 35:1, 25:1, 15:1 and 5:1, respectively collecting the eluted liquid, and measuring to obtain bitter gingko phenolic acid;
s3: preparing rheum officinale extract: pulverizing radix et rhizoma Rhei, extracting with water under reflux, concentrating the extractive solution to obtain concentrated solution, adding 78% ethanol, and extracting under reflux to obtain radix et rhizoma Rhei extract;
s4: preparing an anti-adhesive coating with tea saponin as a main component: mixing 65 parts of tea saponin, 30 parts of polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract uniformly in parts by weight; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
Example 4
An anti-adhesive coating taking tea saponin as a main component comprises, by weight, 70 parts of tea saponin, 25 parts of polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
The preparation method of the anti-sticking coating with the tea saponin as the main component comprises the following steps:
s1: extracting tea-oil camellia saponin: pulverizing oil tea cake, extracting with 80% ethanol, and concentrating the extractive solution to obtain concentrated solution; gradient eluting the concentrated solution by adopting a polyamide chromatographic column, and respectively collecting and measuring the eluted liquid to obtain the sasanqua saponin; the eluent used was water, 30% ethanol, 50% ethanol, 70% ethanol, 90% ethanol and 95% ethanol.
S2: extracting ginkgolic acid: crushing bitter gingko, adding water for dissolution, adopting a macroporous adsorption resin column to perform gradient elution on the dissolution liquid by using 30% and 78% ethanol, recovering the eluent, drying and concentrating, then adopting a silica gel column for elution, sequentially performing gradient elution by using petroleum ether-ethyl acetate with the volume ratio of 45:1, 35:1, 25:1, 15:1 and 5:1, respectively collecting the eluted liquid, and measuring to obtain bitter gingko phenolic acid;
s3: preparing rheum officinale extract: pulverizing radix et rhizoma Rhei, extracting with water under reflux, concentrating the extractive solution to obtain concentrated solution, adding 78% ethanol, and extracting under reflux to obtain radix et rhizoma Rhei extract;
s4: preparing an anti-adhesive coating with tea saponin as a main component: mixing oil tea saponin 70 parts, polypropylene 25 parts, ginkgolic acid, rheum officinale extract and ootheca Mantidis lipid extract uniformly in parts by weight; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
Example 5
An anti-adhesive coating taking tea saponin as a main component comprises, by weight, 75 parts of tea saponin, 20 parts of polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
The preparation method of the anti-sticking coating with the tea saponin as the main component comprises the following steps:
s1: extracting tea-oil camellia saponin: pulverizing oil tea cake, extracting with 80% ethanol, and concentrating the extractive solution to obtain concentrated solution; gradient eluting the concentrated solution by adopting a polyamide chromatographic column, and respectively collecting and measuring the eluted liquid to obtain the sasanqua saponin; the eluent used was water, 30% ethanol, 50% ethanol, 70% ethanol, 90% ethanol and 95% ethanol.
S2: extracting ginkgolic acid: crushing bitter gingko, adding water for dissolution, adopting a macroporous adsorption resin column to perform gradient elution on the dissolution liquid by using 30% and 78% ethanol, recovering the eluent, drying and concentrating, then adopting a silica gel column for elution, sequentially performing gradient elution by using petroleum ether-ethyl acetate with the volume ratio of 45:1, 35:1, 25:1, 15:1 and 5:1, respectively collecting the eluted liquid, and measuring to obtain bitter gingko phenolic acid;
s3: preparing rheum officinale extract: pulverizing radix et rhizoma Rhei, extracting with water under reflux, concentrating the extractive solution to obtain concentrated solution, adding 78% ethanol, and extracting under reflux to obtain radix et rhizoma Rhei extract;
s4: preparing an anti-adhesive coating with tea saponin as a main component: mixing oil tea saponin 75 parts, polypropylene 20 parts, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract uniformly in parts by weight; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
Example 6
An anti-adhesive coating taking tea saponin as a main component comprises, by weight, 80 parts of tea saponin, 15 parts of polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
The preparation method of the anti-sticking coating with the tea saponin as the main component comprises the following steps:
s1: extracting tea-oil camellia saponin: pulverizing oil tea cake, extracting with 80% ethanol, and concentrating the extractive solution to obtain concentrated solution; gradient eluting the concentrated solution by adopting a polyamide chromatographic column, and respectively collecting and measuring the eluted liquid to obtain the sasanqua saponin; the eluent used was water, 30% ethanol, 50% ethanol, 70% ethanol, 90% ethanol and 95% ethanol.
S2: extracting ginkgolic acid: crushing bitter gingko, adding water for dissolution, adopting a macroporous adsorption resin column to perform gradient elution on the dissolution liquid by using 30% and 78% ethanol, recovering the eluent, drying and concentrating, then adopting a silica gel column for elution, sequentially performing gradient elution by using petroleum ether-ethyl acetate with the volume ratio of 45:1, 35:1, 25:1, 15:1 and 5:1, respectively collecting the eluted liquid, and measuring to obtain bitter gingko phenolic acid;
s3: preparing rheum officinale extract: pulverizing radix et rhizoma Rhei, extracting with water under reflux, concentrating the extractive solution to obtain concentrated solution, adding 78% ethanol, and extracting under reflux to obtain radix et rhizoma Rhei extract;
s4: preparing an anti-adhesive coating with tea saponin as a main component: mixing 80 parts of tea saponin, 15 parts of polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract uniformly in parts by weight; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
Comparative example 1
An anti-adhesive coating comprises, by weight, 20 parts of polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
The preparation method of the anti-adhesive coating comprises the following steps:
s1: extracting ginkgolic acid: crushing bitter gingko, adding water for dissolution, adopting a macroporous adsorption resin column to perform gradient elution on the dissolution liquid by using 30% and 78% ethanol, recovering the eluent, drying and concentrating, then adopting a silica gel column for elution, sequentially performing gradient elution by using petroleum ether-ethyl acetate with the volume ratio of 45:1, 35:1, 25:1, 15:1 and 5:1, respectively collecting the eluted liquid, and measuring to obtain bitter gingko phenolic acid;
s2: preparing rheum officinale extract: pulverizing radix et rhizoma Rhei, extracting with water under reflux, concentrating the extractive solution to obtain concentrated solution, adding 78% ethanol, and extracting under reflux to obtain radix et rhizoma Rhei extract;
s3: preparing an anti-adhesive coating: mixing polypropylene 20 parts, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract uniformly according to parts by weight; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
Comparative example 2
An anti-adhesive coating comprises, by weight, 75 parts of tea saponin, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
The preparation method of the anti-adhesive coating comprises the following steps:
s1: extracting tea-oil camellia saponin: pulverizing oil tea cake, extracting with 80% ethanol, and concentrating the extractive solution to obtain concentrated solution; gradient eluting the concentrated solution by adopting a polyamide chromatographic column, and respectively collecting and measuring the eluted liquid to obtain the sasanqua saponin; the eluent used was water, 30% ethanol, 50% ethanol, 70% ethanol, 90% ethanol and 95% ethanol.
S2: extracting ginkgolic acid: crushing bitter gingko, adding water for dissolution, adopting a macroporous adsorption resin column to perform gradient elution on the dissolution liquid by using 30% and 78% ethanol, recovering the eluent, drying and concentrating, then adopting a silica gel column for elution, sequentially performing gradient elution by using petroleum ether-ethyl acetate with the volume ratio of 45:1, 35:1, 25:1, 15:1 and 5:1, respectively collecting the eluted liquid, and measuring to obtain bitter gingko phenolic acid;
s3: preparing rheum officinale extract: pulverizing radix et rhizoma Rhei, extracting with water under reflux, concentrating the extractive solution to obtain concentrated solution, adding 78% ethanol, and extracting under reflux to obtain radix et rhizoma Rhei extract;
s4: preparing an anti-adhesive coating with tea saponin as a main component: mixing oil tea saponin 75 parts, ginkgolic acid, rheum officinale extract and ootheca Mantidis lipid extract uniformly according to parts by weight; wherein the total content of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5 parts.
Comparative example 3
The anti-sticking coating comprises 75 parts of tea saponin and 20 parts of polypropylene in parts by weight.
The preparation method of the anti-adhesive coating comprises the following steps:
s1: extracting tea-oil camellia saponin: pulverizing oil tea cake, extracting with 80% ethanol, and concentrating the extractive solution to obtain concentrated solution; gradient eluting the concentrated solution by adopting a polyamide chromatographic column, and respectively collecting and measuring the eluted liquid to obtain the sasanqua saponin; the eluent used was water, 30% ethanol, 50% ethanol, 70% ethanol, 90% ethanol and 95% ethanol.
S2: preparing an anti-adhesive coating with tea saponin as a main component: and (3) uniformly mixing 75 parts of tea saponin and 20 parts of polypropylene according to parts by weight.
Effect example 1
Minimum Inhibitory Concentration (MIC) determination of anti-stickness coating on bacillus cereus:
determining the minimum inhibitory concentration by adopting a double gradient dilution method, and carrying out gradient dilution by using a culture medium; the bacillus cereus with the indicating bacteria in the logarithmic phase is diluted to 1X 106cfu/mL by using NB culture medium in a gradient manner, 100 mu L of the bacterial liquid is respectively taken in 1 st-6 th holes of a 24-hole plate, 2mL of anti-sticking coating prepared in examples 1-6 are added into each hole, 100 mu L of NB culture medium and 2mL of culture medium are added into 7 th holes to serve as negative blank control, 2mL of culture medium is added into 8 th holes to serve as blank control, the process is completed within 15min, three parallel processes are carried out, the average value is obtained, wherein the abscissa is the weight ratio of the tea saponin in the anti-sticking coating taking the tea saponin as a main component, and the ordinate is the light absorption value.
Mixing, placing 24 pore plate in incubator at 37deg.C for culturing for 18-24 hr, taking out, stirring, and measuring OD with enzyme-labeled instrument 600 The method comprises the steps of carrying out a first treatment on the surface of the Takes the concentration of the saponin of the tea-oil tree as the abscissa and takes the OD 600 The value is plotted on the ordinate, and the inflection point is the minimum inhibitory concentration.
Bacteriostasis%= (ODr-OD/ODr-ODb) ×100% ODr: the absorbance of the positive control group, ODb, negative control group and OD, oil tea saponin group.
The bacteriostatic effect of the release coatings prepared in examples 1-6 is shown in figure 1.
Analysis of results:
according to the result of the formula, the negative control experiment OD 600 As shown in fig. 1, the absorbance value is 0.200±0.05, and the oil tea saponin prepared in example 5 comprises, by weight, 75 parts of oil tea saponin, 20 parts of polypropylene, ginkgolic acid, rheum officinale extract and ootheca Mantidis lipid extract; wherein, 5 parts of ginkgolic acid, rheum officinale extract and ootheca Mantidis lipid extract are used as the total components, and the obtained anti-adhesion coating has the best antibacterial effect; the absorbance in example 5 was less than that of the negative control, demonstrating that bacterial growth was inhibited, and the anti-sticking coating of example 5, which uses tea saponin as the major ingredient, had better inhibition on bacillus cereus.
Effect example 2
Inhibition test of release coating on bacillus cereus biofilm formation:
measuring the cell envelope of the bacillus cereus, and adopting a crystal violet staining semi-quantitative method; the Bacillus cereus strain with logarithmic phase is diluted to 1×10 in gradient with NB medium 6 cfu/mL and 1X 10 8 cfu/mL of two bacterial suspensions; diluting the anti-adhesion coating prepared in example 5 and taking the sasanqua saponin as a main component respectively to obtain final concentrations of MIC, 1/2MIC, 1/4MIC and 1/8MIC, adding the anti-adhesion coating with the concentrations of MIC, 1/2MIC, 1/4MIC and 1/8MIC into a culture medium containing bacterial suspension, and adding normal saline into the culture medium by a negative control group; first immersing needle-shaped pore plate cover into bacterial suspensionCulturing culture medium with anti-adhesion coating of different concentrations at 37deg.C for 24 hr, taking out needle-shaped pore plate cover, immersing in sterilized physiological saline, immersing needle-shaped pore plate cover in crystal violet solution for 30min, immersing needle-shaped pore plate cover in sterilized physiological saline again for cleaning, immersing needle-shaped pore plate cover in ethanol for 15min, sucking out crystal violet, and detecting OD with spectrophotometer 600 Performing three groups of parallel tests on the lower absorbance value; wherein, the abscissa is the anti-adhesive coating with different concentrations, and the ordinate is the light absorption value.
Analysis of results: from fig. 2 and 3, it can be seen that the anti-adhesion coatings with different concentrations prepared by the application have obvious antibacterial effect relative to the blank test.
Effect example 3
Anti-sticking coating inhibition test on bacillus cereus:
bacterial suspension culture: culturing bacillus cereus in an NB culture medium, and cleaning the bacillus cereus by using a phosphate buffer solution containing 2% of peptone in parts by weight and 0.05mol/L to prepare a bacterial suspension; bacteriostasis test: taking a filter paper sheet, beating the filter paper into a round paper sheet by using a puncher with the length of 0.5cm, respectively dripping 6 mu L of the anti-sticking coating obtained in the examples 1-6 and the anti-sticking coating prepared in the comparative examples 1-3 on the paper sheet by using a liquid-transferring gun, and preparing a sample sheet after full absorption; sucking 100 mu L of the bacterial suspension onto a TSC agar medium, and uniformly coating 3 times by using a coater; lightly sticking a sample on a culture plate by using sterile forceps, taking normal saline as a blank control, culturing for 24 hours in a constant temperature incubator at 37 ℃, and measuring the diameter of each treated colony by using a caliper with the unit of mm; the diameters were measured vertically by the crisscross method each time, and the test was repeated 3 times to obtain an average value.
The hypha growth inhibition rate was calculated according to the following formula:
hypha inhibition (%) = (control colony growth diameter-treated colony growth diameter)/control colony growth diameter ×100
The inhibitory effect of the release coating on bacillus cereus is shown in table 1:
table 1: anti-sticking coatings prepared in examples 1-6, comparative examples 1-3 and control group had inhibitory effects on bacillus cereus;
inhibition of bacillus cereus (%)
Control group 20.1
Example 1 60.5
Example 2 65.1
Example 3 72.3
Example 4 77.5
Example 5 90.5
Example 6 76.3
Comparative example 1 30.2
Comparative example 2 86.6
Comparative example 3 85.1
The results in Table 1 show that the anti-sticking coating prepared in example 5 has higher inhibition activity on bacillus cereus; comprises 75 parts of tea saponin, 20 parts of polypropylene, ginkgolic acid, rheum officinale extract and ootheca mantidis lipid extract in parts by weight; wherein, 5 parts of ginkgolic acid, rheum officinale extract and ootheca Mantidis lipid extract are used as the total components, and the obtained anti-adhesion coating has the best antibacterial effect; from comparative example 1, it can be seen that the antibacterial effect is poor without adding the tea saponin, which shows that the tea saponin plays a main role in inhibiting bacillus cereus in the prepared anti-sticking coating.
The design focus of the invention is that natural oil tea saponin is adopted to inhibit food-borne pathogenic bacillus cereus, so that during food production, not only is attention paid to food sterilization enhanced, but also anti-adhesive coatings are coated on corner pipelines which are ignored by food machinery, thereby reducing food poisoning phenomena such as vomiting and diarrhea caused by creating a comfortable living environment for bacteria to generate biofilm and adhere to the food.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so any minor modifications, equivalent changes and modifications made to the above embodiments according to the technical principles of the present invention still fall within the scope of the technical solutions of the present invention.

Claims (8)

1. An anti-adhesive coating taking tea-oil saponin as a main component is characterized in that; comprises 55-80 parts of tea saponin, 15-30 parts of polypropylene, 2-3 parts of ginkgolic acid, 1-2 parts of rheum officinale extract and 0.5-1 part of ootheca mantidis lipid extract in parts by weight; the oil tea saponin is extracted from a byproduct oil tea cake obtained after oil tea seed oil extraction, and the process for extracting the oil tea saponin from the oil tea cake comprises ethanol extraction and polyamide chromatographic column extraction.
2. The anti-sticking coating based on tea saponin as claimed in claim 1, wherein the anti-sticking coating comprises the following components; 75 parts of tea-oil camellia saponin.
3. The anti-sticking coating based on tea saponin as claimed in claim 1, wherein the anti-sticking coating comprises the following components; the total weight percentage of the ginkgolic acid, the rheum officinale extract and the ootheca Mantidis lipid extract is 5%.
4. A process for the preparation of an anti-adhesion coating based on tea-oil saponin as defined in any one of claims 1 to 3, characterized in that; the method comprises the following steps:
s1: extracting tea-oil camellia saponin: pulverizing oil tea cake, extracting with 80% ethanol, and concentrating the extractive solution to obtain concentrated solution; gradient eluting the concentrated solution by adopting a polyamide chromatographic column, and respectively collecting and measuring the eluted liquid to obtain the sasanqua saponin;
s2: extracting ginkgolic acid: crushing bitter gingko, adding water for dissolution, adopting a macroporous adsorption resin column to perform gradient elution on the dissolution liquid by using 30% and 78% ethanol, recovering the eluent, drying and concentrating, then adopting a silica gel column for elution, sequentially performing gradient elution by using petroleum ether-ethyl acetate with the volume ratio of 45:1, 35:1, 25:1, 15:1 and 5:1, respectively collecting the eluted liquid, and measuring to obtain bitter gingko phenolic acid;
s3: preparing rheum officinale extract: pulverizing radix et rhizoma Rhei, extracting with water under reflux, concentrating the extractive solution to obtain concentrated solution, adding 60% -78% ethanol, and extracting under reflux to obtain radix et rhizoma Rhei extract;
s4: preparing an anti-adhesive coating with tea saponin as a main component: according to the weight portions, 55 to 80 portions of tea saponin, 15 to 30 portions of polypropylene, 2 to 3 portions of ginkgolic acid, 1 to 2 portions of rheum officinale extract and 0.5 to 1 portion of ootheca mantidis lipid extract are evenly mixed.
5. The method for preparing the anti-sticking coating with tea saponin as the main component according to claim 4, wherein the method comprises the following steps of; the eluent adopted in the S1 is water, 30% ethanol, 50% ethanol, 70% ethanol, 90% ethanol and 95% ethanol.
6. Use of the anti-adhesion coating based on tea-oil camellia saponin as claimed in any one of claims 1-3 for inhibiting bacillus cereus, wherein the anti-adhesion coating based on tea-oil camellia saponin is used for inhibiting bacillus cereus in food.
7. The application of the anti-adhesion coating taking the tea saponin as a main component in inhibiting bacillus cereus as claimed in claim 6, wherein the anti-adhesion coating taking the tea saponin as a main component is used for destroying bacillus cereus to adhere to the surface of a carrier, destroying a biological membrane structure and further inhibiting bacillus cereus.
8. The use of an anti-adhesion coating based on tea saponin as defined in claim 6 for inhibiting bacillus cereus, wherein the anti-adhesion coating based on tea saponin is applied to a pipe or corner of a food processing device.
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