Slow-release essential oil natural preservative and preparation method thereof

Abstract

The invention discloses a slow-release essential oil natural preservative, which comprises plant essential oil, beta-cyclodextrin, starch and an activator, the plant essential oil is a core material, the beta-cyclodextrin is a wall material, the plant essential oil is one or two of mustard essential oil, garlic essential oil, cumin essential oil and mint essential oil, and the combination ratio is 1: 0-3. The starch is activated by using the principle of electron beam irradiation of free radicals, and is used for a beta cyclodextrin-essential oil embedding system, so that the subsequent irradiation grafting link and the water washing and alcohol washing link in an acrylamide system are omitted, and the process is simpler and more efficient.

Description

Technical Field

[0001] The invention relates to the technical field of natural preservatives, and in particular to a sustained-release essential oil natural preservative and a preparation method thereof. Background Art

[0002] Plant essential oils are composed of terpenes, ketones, epoxy compounds, esters, acids, alcohols and sulfides, and have good antibacterial, antiviral and antioxidant effects. Plant essential oils are secondary metabolites of the plant itself, with good environmental compatibility, not easy to produce resistance, broad-spectrum bactericidal and insecticidal, sterilization, and can be widely used in food, medical, cosmetics and other fields. For example, clove essential oil has a strong inhibitory effect on pathogenic microorganisms such as Escherichia coli, Staphylococcus aureus, Candida albicans, Pseudomonas aeruginosa, and Salmonella. However, as a liquid volatile aromatic component, essential oil is easy to volatilize and has poor stability, resulting in high storage and transportation requirements and poor convenience of use, which greatly limits the application of essential oil products. In order to improve the storage and transportation and usability of essential oil products, essential oils are often prepared into sustained-release solid dosage forms by embedding. There are two main sustained-release technologies: microencapsulation technology and cyclodextrin and its derivative inclusion technology. However, there are still some technical bottlenecks in microencapsulation technology that need to be overcome. For example, the mechanical strength of natural compound wall materials is relatively weak. It is necessary to screen wall materials with strong stability, good film-forming effect, environmental protection, low toxicity, high mechanical strength and low cost to obtain nano-microcapsule materials with more application value. The common method of use is the inclusion technology of cyclodextrin and its derivatives. The use of β-cyclodextrin to embed improves the stability of the target, prevents the escape of volatile components, increases the solubility of poorly soluble substances, and improves the utilization efficiency. After making solid dosage products, essential oils are used for volatilization and antibacterial inhibition. There is no need to contact the product, which is convenient and quick to use. However, β-cyclodextrin has limited effects on hydrophobic regions and catalytic activity, so it is necessary to modify β-cyclodextrin or find its derivatives with better performance. For this reason, we propose a sustained-release essential oil natural preservative and its preparation method. Summary of the invention

[0003] In order to solve the above problems, the present invention provides a sustained-release essential oil natural preservative and a preparation method thereof.

[0004] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: a sustained-release essential oil natural preservative comprises plant essential oil, β-cyclodextrin, starch and an activator, wherein the plant essential oil is a core material, the β-cyclodextrin is a wall material, the plant essential oil is 1-2 of mustard essential oil, garlic essential oil, cumin essential oil and peppermint essential oil, and the combination ratio is 1:0-3.

[0005] In the above scheme, the activator is one or two of black pepper, pepper, linolenic acid, linoleic acid, cysteine, alanine, calcium succinate, and calcium glycinate.

[0006] In the above scheme, the ratio of the activator to the starch is 1:50-300.

[0007] In the above scheme, the preservative is composed of the following raw materials in parts by weight: starch, essential oil, and β-cyclodextrin in a ratio of 1:10-15:70-100.

[0008] A slow-release essential oil natural preservative comprises the following steps:

[0009] Step S1, starch activation treatment: electron beam irradiation, irradiation dose of 0.5-6 kGy, electron beam energy of 10 MeV, irradiation non-uniformity of 1.1-1.5, electron beam irradiation repetition scanning frequency of 80-630 pps, scanning width of 600-800 mm, adding activator and mixing before irradiation;

[0010] Step S2, starch gelatinization: dissolving starch in water to make the concentration of starch aqueous solution 0.1-0.3 g / mL, gelatinization temperature 65-85° C., stirring speed 200 rpm, gelatinization time 20-30 min;

[0011] Step S3, preparing a saturated aqueous solution of β-cyclodextrin;

[0012] Step S4, slow-release agent mixed precipitation: add plant essential oil to the prepared starch gelatinization solution, the temperature is 60±5°C, the stirring speed is 200rpm, then add the mixed solution to the saturated aqueous solution of β-cyclodextrin, the blend is stirred at a reaction temperature of 50-70°C, the reaction time is 2-4h, and the stirring speed is 400-600rpm to produce precipitation;

[0013] Step S5, preparing inclusion compound: filtering the precipitate produced in step 4, and drying in vacuo at 45° C. to obtain plant essential oil / β-cyclodextrin-starch inclusion compound.

[0014] Compared with the prior art, the invention has the following beneficial effects: the slow-release essential oil natural preservative and its preparation method are more efficient and have a higher product yield than β-cyclodextrin-essential oil. Starch is activated by the principle of electron beam irradiation free radicals and used in the β-cyclodextrin-essential oil embedding system, omitting the subsequent irradiation grafting link and the water washing and alcohol washing link in the acrylamide system, making the process simpler and more efficient. DETAILED DESCRIPTION

[0015] The following will be described clearly and completely in conjunction with the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0016] A sustained-release essential oil natural preservative comprises plant essential oil, beta-cyclodextrin, starch and an activator, wherein the plant essential oil is a core material, the beta-cyclodextrin is a wall material, and the plant essential oil is one to two of mustard essential oil, garlic essential oil, cumin essential oil and peppermint essential oil, with a combination ratio of 1:0-3.

[0017] The activator is one or two of black pepper, pepper, linolenic acid, linoleic acid, cysteine, alanine, calcium succinate, and calcium glycinate.

[0018] The ratio of the activator to the starch is 1:50-300.

[0019] The preservative is composed of the following raw materials in parts by weight: starch, essential oil, beta-cyclodextrin system in a ratio of 1:10-15:70-100.

[0020] A method for preparing a sustained-release essential oil natural preservative comprises the following steps:

[0021] Step S1, starch activation treatment: electron beam irradiation, irradiation dose of 0.5-6 kGy, electron beam energy of 10 MeV, irradiation non-uniformity of 1.1-1.5, electron beam irradiation repetition scanning frequency of 80-630 pps, scanning width of 600-800 mm, adding activator and mixing before irradiation;

[0022] Step S2, starch gelatinization: dissolving starch in water to make the concentration of starch aqueous solution 0.1-0.3 g / mL, gelatinization temperature 65-85° C., stirring speed 200 rpm, gelatinization time 20-30 min;

[0023] Step S3, preparing a saturated aqueous solution of β-cyclodextrin;

[0024] Step S4, slow-release agent mixed precipitation: add plant essential oil to the prepared starch gelatinization solution, the temperature is 60±5°C, the stirring speed is 200rpm, then add the mixed solution to the saturated aqueous solution of β-cyclodextrin, the blend is stirred at a reaction temperature of 50-70°C, the reaction time is 2-4h, and the stirring speed is 400-600rpm to produce precipitation;

[0025] Step S5, preparing inclusion compound: filtering the precipitate produced in step 4, and drying in vacuo at 45° C. to obtain plant essential oil / β-cyclodextrin-starch inclusion compound.

[0026] Specifically, in the present invention, the activator is mustard essential oil as an example, starch and the activator are uniformly mixed, electron beam irradiation, the irradiation dose is 0.5kGy, the electron beam energy is 10MeV, the irradiation non-uniformity is 1.1, the electron beam irradiation repetition scanning frequency is 80pps, the scanning width is 600mm, and the starch and the activator are dissolved in water after irradiation, so that the concentration of the starch aqueous solution is 0.1g / mL, the gelatinization temperature is 65°C, the stirring speed is 200rpm, and the gelatinization time is 20. Add plant essential oil to the prepared starch gelatinization solution, the temperature is 60±5°C, the stirring speed is 200rpm, and then the mixed solution is added to the saturated aqueous solution of β-cyclodextrin, the blend is stirred at a reaction temperature of 50°C, the reaction time is 2h, and the stirring speed is 400rpm to produce precipitation. The precipitate produced by suction filtration 4 is vacuum dried at 45°C to obtain a plant essential oil / β-cyclodextrin-starch inclusion compound.

[0027] Mode 1 is a common embedding system, β-cyclodextrin / essential oil system; Mode 2 is the system of the present invention, starch / β-cyclodextrin / essential oil system.

[0028]

[0029] Experiment on the preservation effect of preservatives on food: The quality control of aquatic products should be based on the total number of colonies not exceeding 5×10 6 CFU / g is the standard. Taking fresh salmon as an example, when the preservative of the present invention is used, the coliform group is less than 10 after refrigeration at 4°C for 6 days. 2 MPN / g, total colony count less than 10 5 CFU / g, it can be considered that the product quality is well maintained. The hardness of the control salmon meat decreased significantly due to bacterial growth, and the hardness of the salmon meat treated with preservatives was not significantly different from the initial value.

[0030] Table 2 Preservation effect of fresh salmon at 4℃ for 9 days

[0031]

[0032] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A sustained-release essential oil natural preservative, characterized in that: The invention comprises plant essential oil, beta-cyclodextrin, starch and an activator, wherein the plant essential oil is a core material, the beta-cyclodextrin is a wall material, the plant essential oil is 1-2 of mustard essential oil, garlic essential oil, cumin essential oil and peppermint essential oil, and the combination ratio is 1:0-3.

2. A sustained-release essential oil natural preservative according to claim 1, characterized in that: The activator is one or two of black pepper, pepper, linolenic acid, linoleic acid, cysteine, alanine, calcium succinate, and calcium glycinate.

3. A sustained-release essential oil natural preservative according to claim 2, characterized in that: The ratio of the activator to the starch is 1:50-300.

4. A sustained-release essential oil natural preservative according to claim 1, characterized in that: The preservative is composed of the following raw materials in parts by weight: starch, essential oil, beta-cyclodextrin system in a ratio of 1:10-15:70-100.

5. The method for preparing a sustained-release essential oil natural preservative according to claim 1, characterized in that: The following steps are involved: Step S1, starch activation treatment: electron beam irradiation, irradiation dose of 0.5-6 kGy, electron beam energy of 10 MeV, irradiation non-uniformity of 1.1-1.5, electron beam irradiation repetition scanning frequency of 80-630 pps, scanning width of 600-800 mm, adding activator and mixing before irradiation; Step S2, starch gelatinization: dissolving starch in water to make the concentration of starch aqueous solution 0.1-0.3 g / mL, gelatinization temperature 65-85° C., stirring speed 200 rpm, gelatinization time 20-30 min; Step S3, preparing a saturated aqueous solution of β-cyclodextrin; Step S4, slow-release agent mixed precipitation: add plant essential oil to the prepared starch gelatinization solution, the temperature is 60±5°C, the stirring speed is 200rpm, then add the mixed solution to the saturated aqueous solution of β-cyclodextrin, the blend is stirred at a reaction temperature of 50-70°C, the reaction time is 2-4h, and the stirring speed is 400-600rpm to produce precipitation; Step S5, preparing inclusion compound: filtering the precipitate produced in step 4, and drying in vacuo at 45° C. to obtain plant essential oil / β-cyclodextrin-starch inclusion compound.

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