CN114601750A

CN114601750A - Preservative composition for oral cleaning and nursing products and preparation method and application thereof

Info

Publication number: CN114601750A
Application number: CN202210184579.6A
Authority: CN
Inventors: 白燕; 孟璐; 刘彦婷; 严峰; 徐亚霞; 李辉; 习娟
Original assignee: Shaanxi Chemical Research Institute Co ltd
Current assignee: Shaanxi Chemical Research Institute Co ltd
Priority date: 2022-02-28
Filing date: 2022-02-28
Publication date: 2022-06-10

Abstract

The invention discloses an antiseptic composition for oral cleaning and nursing products, which comprises the following raw materials in parts by weight, based on 100 parts by weight: 3-35 parts of a preservative A, 1-36 parts of a preservative B, 0.1-15 parts of a synergist, 0.02-10 parts of a stabilizer and 4-70 parts of a solvent; wherein the preservative A is any one or more of benzoic acid, sodium benzoate, phenoxyethanol, sorbic acid and sodium sorbate; the preservative B is any one or more of chlorphenesin, 4-hydroxybenzoic acid, methyl 4-hydroxybenzoate, ethyl 4-hydroxybenzoate, propyl 4-hydroxybenzoate, dehydroacetic acid, sodium dehydroacetate and benzyl alcohol. Meanwhile, the invention also discloses a preparation method and application of the preservative composition. The preservative composition for the oral cleaning and nursing product provided by the invention is good in stability, excellent in preservative property and high in safety.

Description

Preservative composition for oral cleaning and nursing products and preparation method and application thereof

Technical Field

The invention belongs to the technical field of preparation of auxiliary preparations of daily necessities, and particularly relates to a preservative composition for an oral cleaning and nursing product, and a preparation method and application thereof.

Background

The oral cleaning and nursing product is used as an oral hygiene product, is closely contacted with the oral cavity in the using process, and is easy to cause human body discomfort if the microorganism indexes do not reach the standard. Therefore, the national has higher sanitary requirements on the oral cleaning and nursing product, for example, the total number of bacterial colonies is required to be less than or equal to 500 CFU/mL, the total number of mould and yeast is required to be less than or equal to 100 CFU/mL in the sanitary index of the oral cleaning and nursing solution, and faecal coliform bacteria, pseudomonas aeruginosa and staphylococcus aureus are not required to be detected. The sanitary index of the toothpaste is basically the same as that of the oral cleaning care solution, the total number of bacterial colonies is required to be less than or equal to 500 CFU/g, the total number of mould and yeast is required to be less than or equal to 100 CFU/g, and heat-resistant coliform bacteria, pseudomonas aeruginosa and staphylococcus aureus are not required to be detected. Oral cleaning and nursing products, in particular to non-disposable products such as oral cleaning and nursing liquid, toothpaste, tooth powder and the like, are continuously contacted with the external environment, such as water, air, oral cavity and the like, in the using process, so that the risk of microbial pollution is increased, and the sanitation index of the oral cleaning and nursing products before unsealing is ensured to meet the requirement, and the using safety is also ensured in the using process. This places greater demands on the product, and to achieve this, safe and reliable preservative products must be added to the product.

According to the requirement of 'toothpaste raw material standard' adopted by the raw materials for oral cleaning and nursing products, 48 preservatives are allowed to be used. Because the preservatives have certain toxicity, the countries have limited requirements on the preservatives. However, the preservative has limited preservative performance in a limited amount, so that a plurality of preservatives need to be compounded for use, so that the preservative effect is enhanced, and even the use amount is reduced.

Disclosure of Invention

Aiming at the defects of the prior art, the invention discloses an antiseptic composition for an oral cleaning and nursing product, which has excellent antiseptic performance and high safety.

The preservative composition for the oral cleaning and nursing product comprises the following raw materials in parts by weight, based on 100 parts by weight:

3-35 parts of a preservative A,

1-36 parts of preservative B

0.1 to 15 parts of a synergist,

0.02-10 parts of stabilizer

4-70 parts of a solvent;

wherein the preservative A is any one or more of benzoic acid, sodium benzoate, phenoxyethanol, sorbic acid and sodium sorbate;

the preservative B is any one or more of chlorphenesin, 4-hydroxybenzoic acid, methyl 4-hydroxybenzoate, ethyl 4-hydroxybenzoate, propyl 4-hydroxybenzoate, dehydroacetic acid, sodium dehydroacetate and benzyl alcohol;

the synergist is a composition of a synergist A and a synergist B, and the synergist A is any one of neotame, thaumatin, alitame and stevioside; the synergist B is at least one of 2-malic acid and pyridine-3-formic acid.

Preferably, the weight ratio of the synergist A to the synergist B is (0.5-1): (3.5-6.5).

Preferably, the stabilizer is any one or more of beta-cyclodextrin, EDTA-2Na, vitamin E acetate and vitamin C.

Preferably, the solvent is water or/and an alcohol solvent.

Preferably, the alcohol solvent is any one or more of 1, 2-propylene glycol, 1, 3-butylene glycol, methyl propylene glycol and phenoxyethanol.

The preparation method of the preservative composition comprises the following steps:

(1) stirring the solvent, the preservative A and the synergist, and uniformly mixing;

(2) adding a preservative B into the mixture, and stirring and mixing the mixture until a uniform solution is obtained;

(3) adding a stabilizer, stirring and uniformly mixing;

(4) filtering with 400 mesh filter cloth to obtain the final product.

The application of the antiseptic composition in the oral cleaning and nursing product comprises the following steps: is added into oral cavity cleaning and nursing product in 0.01-0.05 wt%.

The invention has the advantages that:

(1) the preservative composition for the oral cleaning and nursing product provided by the invention has good stability, and the preservative composition has no obvious change in appearance after being placed for 4 months at 50 ℃;

(2) the preservative property is excellent, and the preservative is added into the oral cleaning and nursing product according to the proportion of 0.01-0.05%, so that the stability and the service performance of the product are not influenced, and the preservative challenge test can be passed; the preservative performance of the oral cleaning and nursing product is obviously improved by using the combination of the sweetening agents as the synergist, so that the taste of the oral cleaning and nursing product can be improved by improving the preservative performance through the synergism;

(3) the safety is high, the LD50 is more than 2000mg/kg through toxicological safety test, and the composition is extremely safe to human bodies when combined with the use amount.

Detailed Description

Example 1

and (3) preservative A: 8 parts of benzoic acid and 20 parts of phenoxyethanol;

and (3) preservative B: 1 part of chlorphenesin and 3 parts of methyl 4-hydroxybenzoate;

a synergist: 0.5 part of neotame and 6.5 parts of 2-hydroxysuccinic acid;

a stabilizer: 0.1 part of beta-cyclodextrin;

solvent: 56 parts of 1, 3-propanediol and 4.9 parts of water;

(3) adding a stabilizer, stirring and uniformly mixing;

(4) filtering with 400 mesh filter cloth to obtain the final product.

Example 2

and (3) preservative A: 5 parts of sodium benzoate and 26 parts of phenoxyethanol;

and (3) preservative B: 1 part of dehydroacetic acid and 2 parts of propyl 4-hydroxybenzoate;

a synergist: 1 part thaumatin and 6 parts pyridine-3-carboxylic acid;

a stabilizer: 0.5 part of vitamin E acetate;

solvent: 58.5 parts of methyl propylene glycol;

the preservative composition was prepared as in example 1.

Example 3

and (3) preservative A: 28 parts of phenoxyethanol;

and (3) preservative B: 5 parts of 4-hydroxybenzoic acid and 1 part of propyl 4-hydroxybenzoate;

a synergist: 1 part of alitame and 3.5 parts of pyridine-3-formic acid;

a stabilizer: 0.02 part of EDTA-2 Na;

solvent: 61.48 parts of 1, 3-propanediol;

the preservative composition was prepared as in example 1.

Example 4

and (3) preservative A: 20 parts of sorbic acid;

and (3) preservative B: 12 parts of dehydroacetic acid;

a synergist: 0.5 part of stevioside and 4.5 parts of 2-hydroxysuccinic acid;

a stabilizer: 0.02 part of EDTA-2 Na;

solvent: 39 parts of phenoxyethanol and 23.98 parts of 1, 2-propanediol;

the preservative composition was prepared as in example 1.

Example 5

and (3) preservative A: 14 parts of sorbic acid and 6 parts of benzoic acid;

and (3) preservative B: 11 parts of dehydroacetic acid;

a synergist: 1 part of neotame, 1 part of 2-hydroxysuccinic acid and 3 parts of pyridine-3-formic acid;

a stabilizer: 0.02 part of EDTA-2 Na;

solvent: 50 parts of phenoxyethanol, 13.98 parts of 1, 2-propylene glycol;

the preservative composition was prepared as in example 1.

Example 6

and (3) preservative A: 3 parts of sodium sorbate;

and (3) preservative B: 36 parts of sodium dehydroacetate;

a synergist: 0.01 part of neotame and 0.09 part of 2-hydroxysuccinic acid;

a stabilizer: 0.02 part of EDTA-2Na,

solvent: 60.88 parts of water;

the preservative composition was prepared as in example 1.

Example 7

And (3) preservative A: 35 parts of phenoxyethanol;

and (3) preservative B: 1 part of sodium dehydroacetate;

a synergist: 0.3 part of neotame and 1.7 parts of 2-hydroxysuccinic acid;

a stabilizer: 2 parts of EDTA-2 Na;

solvent: 60 parts of 1, 3-butanediol;

the preservative composition was prepared as in example 1.

Example 8

And (3) preservative A: 35 parts of phenoxyethanol;

and (3) preservative B: 30 parts of benzyl alcohol and 6 parts of 4-hydroxyphenyl propyl ester;

a synergist: 2 parts of neotame, 10 parts of 2-hydroxysuccinic acid and 3 parts of pyridine-3-formic acid;

a stabilizer: 10 parts of vitamin C;

solvent: 4 parts of 1, 3-butanediol;

the preservative composition was prepared as in example 1.

Comparative example 1

The same procedure as in example 1 was repeated except that neotame was not included.

Comparative example 2

The same procedure as in example 1 was repeated except that 2-hydroxysuccinic acid was not contained.

Comparative example 3

The synergist was 6.5 parts neotame and 0.5 part 2-hydroxysuccinic acid, otherwise as in example 1.

Stability survey

In order to examine the stability, the preservative compositions prepared in examples and comparative examples were observed to have no significant change in appearance when left at 50 ℃ for 4 months, the preservatives prepared in examples 1 to 8 did not have significant change in appearance, the preservatives of comparative examples 1 to 2 did not have significant change in appearance, and the preservative of comparative example 3 had precipitation.

Second, experiment of corrosion resistance challenge

The self-made mouthwash has the following formula (the total amount is 100%):

the preparation method comprises the following steps: adding menthol into the mixed solution of sorbitol, glycerol and propylene glycol, stirring until the menthol is completely dissolved, finally adding deionized water, continuously stirring until the menthol is clear, standing for 18-36 hours at 3-5 ℃, and filtering to obtain the mouthwash.

The preservative compositions provided in examples 1,3 and comparative examples 1-2 were each added to homemade mouthwash at 0.01%, 0.03%, 0.05% by mass, respectively, and tested for microbial challenge according to the USP27(51) microbial preservative efficacy test standard for testing microbial species as follows: (1) bacteria: pseudomonas aeruginosa (CGMCC 1.2464), Escherichia coli (ATCC 44102), Staphylococcus aureus (CGMCC aureus) CGMCC 1.0089; (2) fungi: candida albicans (CGMCC 2.2086), Aspergillus niger (CGMCC 3.3928). The results are shown in tables 1-4.

Table 1 example 1 corrosion protection challenge results

As can be seen from Table 1, the preservative composition of example 1 had a total bacterial count of 2.2X 10 on day 7 when 0.01% was added³cfu/g, total number of fungi 1.2X 10³cfu/g. Total bacterial count at day 14 was 3.6X 10²cfu/g, total number of fungi 4.1X 10²cfu/g. The total colony number of bacteria and fungi at 14 days is less than 10 of the initial colony number^-3The total bacterial colony numbers of the bacteria and the fungi on the 21 st day are respectively 50 cfu/g and 20 cfu/g, and the total bacterial colony numbers of the bacteria and the fungi on the 28 th day are respectively less than 10 cfu/g, which shows that the preservative system pair of the sample of the example 1The microorganism has excellent inhibition and killing effects and passes challenge tests; from day 7, the self-made mouth wash added with 0.03% and 0.05% of the preservative composition has the bacteria and fungi in the sample less than 10 cfu/g, which shows that the preservative system of the sample has extremely strong inhibition and killing effects on microorganisms and passes the challenge test.

Table 2 example 3 preservative challenge results

As can be seen from Table 2, the preservative composition of example 3 had a total bacterial count of 1.1X 10 on day 7 when 0.01% was added³cfu/g, total number of fungi 2.8X 10³cfu/g, total bacterial count at day 14 of 1.1X 10²cfu/g, total number of fungi 2.1X 10²cfu/g. The total colony number of bacteria and fungi at 14 days is less than 10 of the initial colony number^-3On day 21, the total bacterial and fungal colonies continuously decreased on day 28, and on day 28, the total bacterial and fungal colonies were each less than 10. The preservative system of the sample has good inhibition and killing effects on microorganisms and passes a challenge test. The bacteria and fungi in the samples added with 0.03 percent and 0.05 percent of the preservative composition are less than 10 cfu/g from the 7 th day, which indicates that the preservative system of the samples has extremely strong killing effect on the microorganisms and passes the challenge test.

Table 3 comparative example 1 corrosion challenge results

Table 4 comparative example 2 corrosion challenge results

From tables 3 and 4, it can be seen that the preservatives of comparative example 1 and comparative example 2 have poor preservative efficacy against the home-made mouthwash at the 28 th day when added in the amounts of 0.01%, 0.03% and 0.05%, and both of the total bacterial count and the total fungal count are reduced, and thus the preservatives fail the challenge test.

Claims

1. A preservative composition for use in oral cleaning care products characterized by: the composition comprises the following raw materials in parts by weight, based on 100 parts by weight:

3-35 parts of a preservative A,

1-36 parts of preservative B

0.1 to 15 parts of a synergist,

0.02-10 parts of stabilizer

4-70 parts of a solvent;

2. The preservative composition according to claim 1, wherein: the weight ratio of the synergist A to the synergist B is (0.5-1): (3.5-6.5).

3. The preservative composition according to claim 2, wherein: the stabilizer is any one or more of beta-cyclodextrin, EDTA-2Na, vitamin E acetate and vitamin C.

4. The preservative composition according to claim 3, wherein: the solvent is water or/and alcohol solvent.

5. The preservative composition according to claim 4, wherein: the alcohol solvent is any one or more of 1, 2-propylene glycol, 1, 3-butanediol, methyl propylene glycol and phenoxyethanol.

6. A process for preparing a preservative composition according to claim 1, characterized in that: the method comprises the following steps:

(3) adding a stabilizer, stirring and uniformly mixing;

(4) filtering with 400 mesh filter cloth to obtain the final product.

7. Use of a preservative composition according to claim 1 in an oral cleaning care product characterized in that: the application is that the medicine is added into oral cavity cleaning and nursing articles according to 0.01-0.05 wt%.