阅读说明：本技术 一种水溶性高分子消杀剂及其制备方法 (Water-soluble high-molecular disinfectant and preparation method thereof ) 是由 汪少芸 游力军 王建华 郑智娟 刘旖 钟宝华 韩金志 于 2021-07-21 设计创作，主要内容包括：本发明公开了一种水溶性高分子消杀剂及其制备方法,属于食品安全技术领域。阳离子葡聚糖、2,6-二氨基己酸和环氧氯丙烷在碱性条件下进行交联聚合反应,旋转蒸发干燥后得到A剂,将A剂溶解于水中,得到有效成分A剂溶液；用水溶解氯化镁,得到氯化镁溶液,将氯化镁溶液和无水乙醇混合,得到低温抗凝B剂溶液；将有效成分A剂溶液与低温抗凝B剂溶液混合,得到所述的水溶性高分子消杀剂。该消杀剂,适用于在-20℃～40℃的环境中以喷洒的方式使用,具有高效、低温条件下不结冰的优势,可用于冷链、冷库、食品外包装细菌的消杀。(The invention discloses a water-soluble polymer disinfectant and a preparation method thereof, belonging to the technical field of food safety. Performing cross-linking polymerization reaction on cationic glucan, 2, 6-diaminocaproic acid and epoxy chloropropane under an alkaline condition, performing rotary evaporation and drying to obtain an agent A, and dissolving the agent A in water to obtain an effective component agent A solution; dissolving magnesium chloride with water to obtain a magnesium chloride solution, and mixing the magnesium chloride solution with absolute ethyl alcohol to obtain a low-temperature anticoagulant B agent solution; mixing the solution of the effective component A with the solution of the low-temperature anticoagulation agent B to obtain the water-soluble polymer disinfectant. The sterilizing agent is suitable for being used in a spraying mode in an environment with the temperature of-20-40 ℃, has the advantages of high efficiency and no ice formation under a low temperature condition, and can be used for sterilizing bacteria in cold chains, cold storages and food outer packages.)

1. A preparation method of a water-soluble polymer disinfectant is characterized by comprising the following steps: the method comprises the following steps:

dissolving 1 part of glucan and 2 parts of 2, 3-epoxypropyltrimethylammonium chloride in 20 parts of deionized water, then adding 0.2 part of sodium hydroxide into the deionized water, heating the mixed solution in a water bath at 50 ℃ for 4 hours, rotationally evaporating the mixed solution at 80 ℃, and drying to obtain cationic glucan;

taking 0.5-2 parts of cationic glucan, 2-4 parts of 2, 6-diaminocaproic acid and 0.1-0.5 part of epoxy chloropropane, carrying out cross-linking polymerization reaction under an alkaline condition, carrying out rotary evaporation and drying to obtain an agent A, and dissolving 1.5-3.5 parts of the agent A by using 5-10 parts of water to obtain an effective component agent A solution;

dissolving 0.81-1.296 parts of magnesium chloride by using 3.8-5.4 parts of water to obtain a magnesium chloride solution, and mixing the magnesium chloride solution and absolute ethyl alcohol by a ratio of 9-19: 1 to obtain a low-temperature anticoagulation agent B solution;

when the anticoagulant is used, mixing the effective component A agent solution and the low-temperature anticoagulant B agent solution in a ratio of 1-5: 1-3, and mixing to obtain the water-soluble polymer disinfectant.

2. The method for producing a water-soluble polymer biocide according to claim 1, wherein: and the pH value under the alkaline condition in the step II is 12-14.

3. The method for producing a water-soluble polymer biocide according to claim 1, wherein: the temperature of the cross-linking polymerization reaction is 40-50 ℃, and the time of the cross-linking polymerization reaction is 2-6 h.

4. The method for producing a water-soluble polymer biocide according to claim 1, wherein: and the temperature of the rotary evaporation in the step II is 60-90 ℃.

5. A water-soluble polymer disinfectant prepared by the process according to claim 1.

6. The use of the water-soluble polymeric sterilizer of claim 5 for cold chain food sterilization.

Technical Field

The invention particularly relates to a water-soluble polymer disinfectant and a preparation method thereof, belonging to the technical field of food safety.

Background

Because the disinfection effect of cold chain food is influenced by a plurality of factors such as a disinfectant, a disinfection mode, disinfection action time and the like, the following problems exist in the current low-temperature cold chain food disinfection: (1) the disinfectant is easy to coagulate, difficult to disperse and difficult to fully contact pathogens under the low-temperature condition, the sterilization activity of a disinfection factor is reduced, an ideal disinfection effect is difficult to achieve, and the disinfectant suitable for the low-temperature freezing condition is very little; (2) the existing disinfectant is not suitable for directly disinfecting and sterilizing foods such as fruits, vegetables, meat, aquatic products, meat products and the like; (3) the compounds in the biocide can adversely affect the physical health of personnel working on the site for extended periods of time. Therefore, the development of the cold-chain food outer package sterilizing agent which is safe and efficient and is suitable for being used under low temperature conditions is significant.

Disclosure of Invention

The invention aims to make up for the defects of the prior art and provides a water-soluble polymer sterilizing agent which has the advantages of stable performance, convenient use, easy storage and the like and can effectively solve the problem of sterilization of cold chain food outer packages in the links of production, processing, storage, transportation, circulation, transaction and the like, and a preparation method thereof.

In order to achieve the purpose, the invention adopts the following technical scheme:

a preparation method of a water-soluble polymer disinfectant is characterized by comprising the following steps: the method comprises the following steps:

dissolving 1 part of glucan and 2 parts of 2, 3-epoxypropyltrimethylammonium chloride in 20 parts of deionized water, then adding 0.2 part of sodium hydroxide into the deionized water, heating the mixed solution in a water bath at 50 ℃ for 4 hours, rotationally evaporating the mixed solution at 80 ℃, and drying to obtain cationic glucan;

taking 0.5-2 parts of cationic glucan, 2-4 parts of 2, 6-diaminocaproic acid and 0.1-0.5 part of epoxy chloropropane, carrying out cross-linking polymerization reaction under an alkaline condition, then carrying out rotary evaporation, and drying to obtain an agent A, and dissolving 1.5-3.5 parts of the agent A by using 5-10 parts of water to obtain an effective component agent A solution;

dissolving 0.81-1.296 parts of magnesium chloride by using 3.8-5.4 parts of water to obtain a magnesium chloride solution, and mixing the magnesium chloride solution and absolute ethyl alcohol by a ratio of 9-19: 1 to obtain a low-temperature anticoagulation agent B solution;

when the anticoagulant is used, mixing the effective component A agent solution and the low-temperature anticoagulant B agent solution in a ratio of 1-5: 1-3, and mixing to obtain the water-soluble polymer disinfectant.

Wherein the pH value under the alkaline condition in the step II is 12-14;

the temperature of the cross-linking polymerization reaction is 40-50 ℃, and the time of the cross-linking polymerization reaction is 2-6 h;

and the temperature of the rotary evaporation in the step II is 60-90 ℃.

A water-soluble polymer disinfectant obtained by the method.

The water-soluble polymer disinfectant is applied to cold chain food disinfection.

Compared with the prior art, the invention has the following advantages: the water-soluble polymer sterilizing agent provided by the invention can directly act on low-temperature environments such as cold chains, refrigeration houses and the like and normal temperature, can ensure that the water-soluble polymer sterilizing agent is not solidified above-20 ℃ in the use process in storage and transportation spaces such as cold chain containers, refrigeration houses, food and the like, can permeate the surface layer of an ice layer to the surface of an outer package, can rapidly sterilize bacteria, and has the advantages of high efficiency and no ice formation in the low-temperature environment.

Drawings

FIG. 1 shows the effect of the water-soluble polymeric disinfectant on Staphylococcus aureus in example 1 of the present invention.

FIG. 2 shows the effect of the water-soluble polymer disinfectant on Escherichia coli in example 1 of the present invention.

FIG. 3 shows the effect of the water-soluble polymeric disinfectant on Staphylococcus aureus in example 2 of the present invention.

FIG. 4 shows the effect of the water-soluble polymer disinfectant on Escherichia coli in example 2 of the present invention.

FIG. 5 shows the effect of the water-soluble polymeric disinfectant on Staphylococcus aureus in example 3 of the present invention.

FIG. 6 shows the effect of the water-soluble polymer disinfectant on Escherichia coli in example 3 of the present invention.

FIG. 7 shows the low temperature performance of the water-soluble polymeric biocides of examples 1 to 3 of the present invention in an environment of-20 ℃.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

Example 1

A water-soluble polymer disinfectant is prepared by the following steps:

(1) dissolving 1 part of glucan and 2 parts of 2, 3-epoxypropyltrimethylammonium chloride in 20 parts of deionized water, adding 0.2 part of sodium hydroxide, heating the mixed solution in a water bath at 50 ℃ for 4 hours, rotationally evaporating at 80 ℃, and drying to obtain the cationic glucan.

(2) Adding 0.5 part of cationic glucan, 2 parts of 2, 6-diaminocaproic acid and 0.2 part of epoxy chloropropane into a container, uniformly mixing, adjusting the pH value of the mixed solution to 12, then controlling the solution to carry out crosslinking polymerization reaction at 40 ℃ for 2 hours, carrying out rotary evaporation at 60 ℃ and drying to obtain an effective component A, and dissolving 1.5 parts of the A by 5 parts of water to obtain an A solution.

(3) Dissolving 0.81 parts of magnesium chloride with 4.5 parts of water to obtain a magnesium chloride solution, mixing the magnesium chloride solution with absolute ethyl alcohol in a ratio of 9: 1 to obtain a low-temperature anticoagulation agent B solution.

(4) Performing the reaction between the solution of the effective component A and the solution of the low-temperature anticoagulation agent B in a ratio of 1: 1 to obtain the water-soluble polymer disinfectant provided by the present example.

The effect of the water-soluble polymer disinfectant provided by the embodiment is tested, the test strains are staphylococcus aureus and escherichia coli, and the whole testing process is realized in a super-clean bench sterile environment. Taking out LB agar preserved in an oven at 50 ℃, preparing a disposable culture dish, pouring the LB agar into the culture dish when the LB agar is hot, wherein each dish is about 20mL, placing the culture dish on a clean bench to be naturally cooled to a solidification state, then dropwise adding 10 drops of bacteria liquid with the concentration of 5.3LgCFU/mL by using a pipette, wherein each drop is 10 mu L, and then spraying 250 mu L of the disinfectant provided by the embodiment onto a culture medium by using a spray can, wherein all operations are finished beside an alcohol lamp. Then the culture medium is placed in a constant temperature incubator at 37 ℃ for 10 hours, and finally the growth condition of the colony is observed. As shown in FIGS. 1 and 2, the water-soluble polymer disinfectant provided by this example has a killing rate of 99.9% or more for both Escherichia coli and Staphylococcus aureus.

Example 2

A water-soluble polymer disinfectant is prepared by the following steps:

(1) dissolving 1 part of glucan and 2 parts of 2, 3-epoxypropyltrimethylammonium chloride in 20 parts of deionized water, adding 0.2 part of sodium hydroxide, heating the mixed solution in a water bath at 50 ℃ for 4 hours, rotationally evaporating at 80 ℃, and drying to obtain the cationic glucan.

(2) Adding 1 part of cationic glucan, 3 parts of 2, 6-diaminocaproic acid and 0.5 part of epoxy chloropropane into a container, uniformly mixing, adjusting the pH of the mixed solution to 13, then controlling the solution to carry out crosslinking polymerization reaction at 50 ℃ for 4 hours, carrying out rotary evaporation at 75 ℃ and drying to obtain an effective component A agent, and dissolving 3.2 parts of the A agent by 8 parts of water to obtain an A agent solution.

(3) Dissolving 0.912 parts of magnesium chloride with 3.8 parts of water to obtain a magnesium chloride solution, mixing the magnesium chloride solution with absolute ethyl alcohol in a ratio of 19: 1 to obtain a low-temperature anticoagulation agent B solution.

(4) Mixing an effective component A agent solution and a low-temperature anticoagulation B agent solution in a ratio of 2: 1 to obtain the water-soluble polymer disinfectant provided by the present example.

The effect of the water-soluble polymer disinfectant provided by the embodiment is tested, the test strains are staphylococcus aureus and escherichia coli, and the whole testing process is realized in a super-clean bench sterile environment. Taking out LB agar preserved in an oven at 50 ℃, preparing a disposable culture dish, pouring the LB agar into the culture dish when the LB agar is hot, wherein each dish is about 20mL, placing the culture dish on a clean bench to be naturally cooled to a solidification state, then dropwise adding 10 drops of bacteria liquid with the concentration of 5.3LgCFU/mL by using a pipette, wherein each drop is 10 mu L, and then spraying 250 mu L of the disinfectant provided by the embodiment onto a culture medium by using a spray can, wherein all operations are finished beside an alcohol lamp. Then the culture medium is placed in a constant temperature incubator at 37 ℃ for 10 hours, and finally the growth condition of the colony is observed. As shown in FIGS. 3 and 4, the water-soluble polymer disinfectant provided by this example has a killing rate of 99.9% or more for both Escherichia coli and Staphylococcus aureus.

Example 3

A water-soluble polymer disinfectant is prepared by the following steps:

(1) dissolving 1 part of glucan and 2 parts of 2, 3-epoxypropyltrimethylammonium chloride in 20 parts of deionized water, adding 0.2 part of sodium hydroxide, heating the mixed solution in a water bath at 50 ℃ for 4 hours, rotationally evaporating at 80 ℃, and drying to obtain the cationic glucan.

(2) Adding 2 parts of cationic glucan, 4 parts of 2, 6-diaminocaproic acid and 0.1 part of epoxy chloropropane into a container, uniformly mixing, adjusting the pH of the mixed solution to 14, then controlling the solution to carry out crosslinking polymerization reaction at 45 ℃ for 6 hours, carrying out rotary evaporation at 90 ℃, drying to obtain an effective component A agent, and dissolving 3.5 parts of the A agent by 10 parts of water to obtain an A agent solution.

(3) Dissolving 1.296 parts of magnesium chloride with 5.4 parts of water to obtain a magnesium chloride solution, mixing the magnesium chloride solution with absolute ethyl alcohol in a weight ratio of 9: 1 to obtain a low-temperature anticoagulation agent B solution.

(4) Mixing an effective component A agent solution and a low-temperature anticoagulation B agent solution in a ratio of 5: 3 to obtain the water-soluble polymer disinfectant provided by the present example.

The effect of the water-soluble polymer disinfectant provided by the embodiment is tested, the test strains are staphylococcus aureus and escherichia coli, and the whole testing process is realized in a super-clean bench sterile environment. Taking out LB agar preserved in an oven at 50 ℃, preparing a disposable culture dish, pouring the LB agar into the culture dish when the LB agar is hot, wherein each dish is about 20mL, placing the culture dish on a clean bench to be naturally cooled to a solidification state, then dropwise adding 10 drops of bacteria liquid with the concentration of 5.3LgCFU/mL by using a pipette, wherein each drop is 10 mu L, and then spraying 250 mu L of the disinfectant provided by the embodiment onto a culture medium by using a spray can, wherein all operations are finished beside an alcohol lamp. Then the culture medium is placed in a constant temperature incubator at 37 ℃ for 10 hours, and finally the growth condition of the colony is observed. As shown in FIGS. 5 and 6, the water-soluble polymer disinfectant provided in this example exhibited a killing rate of 99.9% or more for both E.coli and Staphylococcus aureus.

Example 4

10mL of each of the water-soluble polymer sterilizers prepared in examples 1 to 3 was placed in a glass bottle and placed in a refrigerator at-20 ℃ for 24 hours, and then the low-temperature performance of the sterilizer was observed. As shown in fig. 7, the water-soluble polymer biocides provided in examples 1 to 3 of the present invention did not freeze at-20 ℃, indicating that the water-soluble polymer biocides provided by the present invention have good low-temperature performance.

The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.