Agarwood essential oil oral antibacterial spray and preparation method thereof

Abstract

The present invention discloses an agarwood essential oil oral antibacterial spray and a preparation method thereof. The raw materials for preparing the spray include, by weight, 79-81 parts of water; 0.01-0.03 parts of agarwood essential oil; 0.04-0.06 parts of cetylpyridinium chloride; 4-6 parts of glycerin; 0.2-0.4 parts of sodium benzoate; 0.6-0.8 parts of hydrogenated castor oil; 12-14 parts of sorbitol; and 0.4-0.6 parts of xylitol. The preparation method comprises mixing and stirring the raw materials other than the agarwood essential oil for 30 minutes to 1 hour, adding the agarwood essential oil, and continuing to stir and mix for 30 minutes to 1 hour. The agarwood oral antibacterial spray of the present invention meets the requirements of relevant specifications and has an ideal antibacterial effect. It enriches the variety of oral spray products on the market.

Description

Technical Field

[0001] The invention relates to an oral spray, and in particular to an agarwood oral antibacterial spray and a preparation method thereof. Background Art

[0002] The oral cavity, the starting point of the respiratory and gastrointestinal tracts, serves as a gateway connecting the body's internal and external environments. Many bacteria from the external ecosystem continuously enter the oral cavity through daily activities like breathing and eating, where they multiply in the warm, moist environment. Streptococci, Staphylococci, and Lactobacilli can cause various oral diseases, including dental caries, bad breath, and gingivitis. Summary of the Invention

[0003] In view of the defects or shortcomings of the existing technology, the present invention provides an agarwood essential oil oral antibacterial spray.

[0004] To this end, the raw materials for preparing the agarwood essential oil oral antibacterial spray provided by the present invention include, by mass, 79-81 parts of water; 0.01-0.03 parts of agarwood essential oil; 0.04-0.06 parts of cetylpyridinium chloride; 4-6 parts of glycerin; 0.2-0.4 parts of sodium benzoate; 0.6-0.8 parts of hydrogenated castor oil; 12-14 parts of sorbitol; and 0.4-0.6 parts of xylitol.

[0005] An optional solution is that the raw materials for preparing the spray further include menthol: 0.02-0.04.

[0006] An optional solution is that the raw materials for preparing the spray further include citric acid: 0.005-0.015.

[0007] An optional solution is that the raw materials for preparing the spray further include trichlorogalactose: 0.006-0.008.

[0008] The present invention also provides a method for preparing the agarwood essential oil oral antibacterial spray. The method comprises mixing and stirring raw materials other than agarwood essential oil for 30 minutes to 1 hour, adding the agarwood essential oil, and continuing to stir and mix for 30 minutes to 1 hour.

[0009] The agarwood oral antibacterial spray of the present invention meets the requirements of relevant regulations and has an ideal antibacterial effect, thereby enriching the variety of oral spray products on the market. DETAILED DESCRIPTION

[0010] Unless otherwise specified, the scientific and technical terms used herein are understood according to the knowledge of ordinary technicians in the relevant fields.

[0011] The following are specific examples provided by the present invention. It should be noted that the raw materials and proportions used in the following examples are intended to illustrate the present invention. Any selections made by those skilled in the art within the scope of the present invention are within the scope of protection of the present invention. The agarwood essential oil used in the following examples was obtained by ethanol extraction. All other raw materials used in the following examples are commercially available and are of cosmetic grade.

[0012] Example 1:

[0013] The formula of the agarwood oral antibacterial spray of this embodiment is shown in Table 1.

[0014] Table 1

[0015]

[0016] The preparation process is as follows: according to the ratio of the formula ingredients shown in Table 1, the components except the agarwood essential oil are placed in a stirring tank, stirred for 1 hour, and then the agarwood essential oil is placed in the stirring tank, mixed with the previous formula ingredients and stirred for 30 minutes, and then weighed and canned to obtain the spray product of this embodiment.

[0017] The spray of this embodiment was further tested for the following indicators:

[0018] 1. pH value

[0019] According to 2.2.1.4 of the 2002 edition of the Technical Specifications for Disinfection; the pH meter model is SevenMulti.

[0020] 2. Heavy metal content

[0021] In accordance with Chapter 4, 1.6 of the 2015 edition of the "Technical Specifications for Safety of Cosmetics"; the ICP / MS (inductively coupled plasma mass spectrometer) model is 7700; the microwave digester model is MultiMave PRO.

[0022] 3. Cetylpyridinium chloride content

[0023] High performance liquid chromatography detection; the high performance liquid chromatograph model is Agilent 1260; the reagents used are: methanol (chromatographic grade), ammonium acetate (analytical grade), glacial acetic acid, and distilled water; the name and concentration of the standard solution are: cetylpyridinium chloride standard solution, with a concentration of 1.0 g / L.

[0024] 4. Toxicology test (acute eye irritation test)

[0025] The acute eye irritation test is based on: Technical Specifications for Disinfection (2002 edition) 2.3.4; the evaluation is based on 6.6(4) of the Regulations for Inspection of Disinfection Products; the specific protocol is as follows:

[0026] 4.1 Experimental Animals

[0027] Animal species: 3 ordinary New Zealand rabbits (purchased from Jianfei Experimental Rabbit Farm, Simen Town, Yuyao City, production license number: SCXK (Zhejiang) 2022-00020); weight range: Animal gender: Both male and female (female animals must be non-pregnant and have not given birth)

[0028] Animal husbandry:

[0029] Animal husbandry: Laboratory Animal Use Permit No.: SYXK(Zhejiang)2021-0032, kept in normal environment, temperature 21.4℃~21.5℃, relative humidity

[0030] Feed source: purchased from Tongxiang Dongfang Feed Co., Ltd., production license number is Zhejiang Feed Certificate (2019) 06708.

[0031] Drinking water: First-grade RO ultrafiltered water (sodium hypochlorite is added to control the free chlorine content in the water to 2-3ppm for sterilization), which is directly provided to animals for free drinking through the drinking nozzle.

[0032] 4.2 Methods:

[0033] Testing basis: Technical Specifications for Disinfection (2002 Edition) 2.3.4; Inspection Regulations for Disinfection Products 6.6(4);

[0034] Pre-examination of experimental animals: 2% sodium fluorescein was used to examine both eyes of the experimental animals within 24 hours before the start of the experiment to exclude animals with eye irritation symptoms, corneal defects and conjunctival damage.

[0035] Operating procedures:

[0036] (1) Gently pull open the lower eyelid of one rabbit eye and drop 0.1 mL of the test sample into the conjunctival sac. The other eye is instilled with normal saline as a normal control.

[0037] (2) After the test sample is instilled, the upper and lower eyelids are passively closed for 4 seconds, and then rinsed with saline after 30 seconds.

[0038] (3) Clinical examination and scoring: The eyes of the animals were examined at 1 h, 24 h, 48 h, 72 h, 7 d, 14 d and 21 d after the instillation of the test substance. The damage and recovery of the conjunctiva, iris and cornea of the rabbits were observed with the naked eye. If no irritation reaction occurred within 72 h, or if the eye irritation reaction was completely recovered on the 7th or 14th day, the test could be terminated early.

[0039] 4.3. Result evaluation method:

[0040] (1) The acute irritation reactions of the rabbit cornea, iris and conjunctiva were scored according to the scoring criteria for eye damage, and the "average score" of corneal damage, iris damage, conjunctival congestion and conjunctival edema was calculated for each animal at three different observation times (24h, 48h and 72h) (i.e., the sum of the scores of each animal at 24h, 48h and 72h divided by the number of observations (3)).

[0041] (2) The average scores and recovery time of corneal, iris and conjunctival congestion and edema of the animals are used to determine the irritation intensity of the test substance to the eyes according to the eye irritation reaction grading standard.

[0042] 5. Microbial indicators

[0043] Based on: Appendix B of GB15979-2002 "Hygienic Standards for Disposable Sanitary Products"; Biochemical Incubator FC222 (200938As6024);

[0044] 6. Antibacterial effect:

[0045] Based on: Appendix C of GB15979-2002 "Hygiene Standards for Disposable Sanitary Products";

[0046] Storage conditions: 90 days in a constant temperature and humidity incubator at 37°C and relative humidity of 80%;

[0047] Test sample: Agarwood essential oil oral antibacterial spray, batch number: 20220728.

[0048] Test strains: Escherichia coli 8099 and Staphylococcus aureus ATCC6538 were provided by the China Industrial Microbiological Culture Collection Center, and were 4-8 generations of fresh slant cultures.

[0049] Test results:

[0050] 1. The average pH value is 4.4;

[0051] 2. Heavy metal content:

[0052] The lead content was 0.18 mg / kg, the arsenic content was <0.0033 mg / kg, and the mercury content was <0.0033 mg / kg. The measurement results are shown in Table 2.

[0053] Table 2

[0054] Test items Test results GB 27954-2020 Limited lead 0.18mg / kg ≤10 mg / kg arsenic <0.0033mg / kg ≤2 mg / kg mercury <0.0033mg / kg ≤1mg / kg

[0055] 3. Cetylpyridinium chloride content

[0056] The average content of cetylpyridinium chloride is 0.490 g / L (the average value of three parallel tests, the test results of each test are: 0.4882 g / L, 0.4966 g / L, and 0.4856 g / L).

[0057] 4. Toxicology test:

[0058] (1) Symptoms of poisoning in animals after exposure: None.

[0059] (2) The average scores of the three animals observed 24h, 48h, and 72h after exposure were: corneal damage <1; iris damage <1; conjunctival congestion <2; and conjunctival edema <2.

[0060] (3) Eye irritation reaction score: See Table 3 below for details. The average score in the table refers to the sum of the 24h, 48h, and 72h scores divided by the number of observation time periods, 3.

[0061] Table 3 Rabbit eye irritation (within 3 days) reaction score

[0062]

[0063]

[0064] As shown in Table 3, according to the criteria for eye irritation reaction of disinfectant products, the test substance has no irritation to the acute eye of rabbits, and the test results meet the requirements of the Technical Specifications for Disinfection (2002 Edition).

[0065] 5. Microbiological testing

[0066] Should The microbial indicators of the agarwood essential oil oral antibacterial spray all met the requirements of GB15979-2002, "Hygiene Standard for Disposable Sanitary Products." The results are shown in Table 4.

[0067] Table 4 Results of microbial indexes of agarwood essential oil oral antibacterial spray

[0068] project result Total bacterial colony count (cfu / ml) <4 coliform group Not detected Pseudomonas aeruginosa Not detected Staphylococcus aureus Not detected Hemolytic Streptococci Not detected Total fungal colonies (cfu / ml) <4

[0069] 6. Antibacterial effect

[0070] After three repeated tests, the results showed that After 90 days of storage, the agarwood essential oil oral antibacterial spray achieved an average inhibition rate of >99.9% against Escherichia coli at 2, 5, 10, and 20 minute exposures. The results are shown in Table 5.

[0071] Table 5 Antibacterial effect of agarwood essential oil oral antibacterial spray on Escherichia coli before and after storage

[0072]

[0073] After three repeated tests, the results showed that after 90 days of storage, the agarwood essential oil oral antibacterial spray of the present invention had an average antibacterial rate of 2 minutes, 5 minutes, 10 minutes, and 20 minutes against Staphylococcus aureus of >99.9%. The results are shown in Table 6.

[0074] Table 6 Antibacterial effect of agarwood essential oil oral antibacterial spray on Staphylococcus aureus before and after storage

[0075]

[0076] The above results show that the agarwood essential oil oral antibacterial spray of the present invention has no obvious changes in appearance and packaging after being stored at 37°C for 90 days; after storage for 90 days, it has a strong antibacterial effect on Escherichia coli and Staphylococcus aureus, and its antibacterial effect is effective for at least 2 years when stored at room temperature, which meets the requirements of GB15979-2002 "Hygiene Standard for Disposable Sanitary Products".

[0077] Example 2:

[0078] Different from Example 1, the formula of the agarwood oral antibacterial spray in this example is shown in Table 7.

[0079] Table 7

[0080]

[0081] Example 3:

[0082] Different from Example 1, the formula of the agarwood oral antibacterial spray in this example is shown in Table 8.

[0083] Table 8

[0084]

[0085] The above description is only a preferred embodiment of the present invention. All equivalent changes and modifications made within the scope of the patent application of the present invention should fall within the scope of the present invention.

Claims

1. An agarwood essential oil oral antibacterial spray, characterized in that: The raw materials for preparing the spray include, by mass, 79-81 parts of water, 0.01-0.03 parts of agarwood essential oil, 0.04-0.06 parts of cetylpyridinium chloride, 4-6 parts of glycerin, 0.2-0.4 parts of sodium benzoate, 0.6-0.8 parts of hydrogenated castor oil, 12-14 parts of sorbitol, 0.4-0.6 parts of xylitol, 0.02-0.04 parts of menthol, 0.005-0.015 parts of citric acid, and 0.006-0.008 parts of trichlorogalactose. The preparation method of the agarwood essential oil oral antibacterial spray comprises: mixing raw materials except the agarwood essential oil and stirring for 30 minutes to 1 hour, adding the agarwood essential oil, and continuing to stir and mix for 30 minutes to 1 hour.

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