CN109568413A - A kind of green plum oral spray and preparation method thereof - Google Patents

A kind of green plum oral spray and preparation method thereof Download PDF

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Publication number
CN109568413A
CN109568413A CN201811602647.6A CN201811602647A CN109568413A CN 109568413 A CN109568413 A CN 109568413A CN 201811602647 A CN201811602647 A CN 201811602647A CN 109568413 A CN109568413 A CN 109568413A
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green plum
parts
oral spray
polyphenol
preparation
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马嫄
罗鸣
徐影平
刘迎佳
袁乙平
殷晓翠
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Xihua University
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/73Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
    • A61K36/736Prunus, e.g. plum, cherry, peach, apricot or almond
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/26Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/0012Galenical forms characterised by the site of application
    • A61K9/0053Mouth and digestive tract, i.e. intraoral and peroral administration
    • A61K9/006Oral mucosa, e.g. mucoadhesive forms, sublingual droplets; Buccal patches or films; Buccal sprays
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/02Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/10Dispersions; Emulsions
    • A61K9/12Aerosols; Foams

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
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  • Engineering & Computer Science (AREA)
  • Epidemiology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Alternative & Traditional Medicine (AREA)
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  • Biotechnology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
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  • Oil, Petroleum & Natural Gas (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Preparation Of Fruits And Vegetables (AREA)
  • Cosmetics (AREA)

Abstract

A kind of green plum oral spray, by 5-10 parts of green plum polyphenol, 1-8 parts of permeation enhancers, 1-5 parts of sweetener, 0-1 parts of preservative, the mass fraction that 76-90 parts of water is formed;Extract green plum polyphenol first: green plum is dry, crushing, sieving, solubilizer extract to obtain green plum polyphenol extract liquor, and extract liquor is concentrated to give green plum polyphenol later;Secondly the green plum polyphenol extract liquor of concentration is dissolved in the water with permeation enhancers, sweetener, is stirred, dispensed after being completely dissolved, sterilize and be made.Green plum oral spray prepared by the present invention has the advantages that spray good effect, raw material sources are wide, at low cost, in good taste.

Description

A kind of green plum oral spray and preparation method thereof
Technical field
The present invention relates to food and its processing technique fields, and in particular to a kind of green plum oral spray and its preparation side Method.
Background technique
As the improvement of people's living standards, saprodontia and periodontitis are gradually spread unchecked, become the most common mouth disease now. Saprodontia is a kind of medical terminology, is commonly called as decayed tooth, decayed tooth, is bacteriosis, therefore it can be with secondary pulpitis and periapical inflammation. It is reported that in most cases, leading to the bacterium of saprodontia is all Gram-negative bacteria, and streptococcus mutans are then most important one Kind.
For preventing for periodontitis, the antibacterials such as clinical research metronidazole, Tinidazole, Tetracyclines, Clindamycin Hydrochloride Chemicals, however chemicals often will cause patient's adverse reaction, therefore researcher starts to probe into natural active matter work It is antibacterial agent to prevent periodontitis, keeps the environment of oral health.Confirm that the natural materials for the treatment of periodontitis are especially more at present, gold Honeysuckle flower, Radix Glycyrrhizae, Chinese yam, peppermint, horseradish, tealeaves etc., and corresponding patent document also has been reported that.Patent document CN102198065A A kind of oral spray and preparation method thereof is disclosed, is mentioned by concentrations such as Siraitia grosvenorii, honeysuckle, Radix Glycyrrhizae, wild chrysanthemum, peppermints Refining, is then mixed with oral spray with other components such as stevia rebaudianum, persimmons.Patent CN201010140223.X discloses one kind Oral spraying agent prepared from Chinese medicine and preparation method thereof, the sweetener side effect in the formula is more and will cause obesity, hypertension, height The health problems such as blood glucose, and the spray curative effect is general, and effect is single, and practicability is poor.Patent 201310209226.8 is public A kind of horseradish oral spray is opened, using horseradish extracting solution as raw material, addition absorption enhancers, corrigent, syrup are the spray Auxiliary material delays throat inflamed sites situation to aggravate, horseradish is current although can effectively inhibit the bacterial growth in oral cavity The special health food of the one kind found in the world, is extremely precious seasoned food in the international market, expensive, because And the oral spray is difficult to popularity.
It is found by investigation, as the green plum of natural antibacterial agent, but there have been no the report for preventing periodontitis.Green plum is also known as fruit Plum, dark plum are that rosaceae apricot belongs to a kind of medicinal and edible plant, native to China, and the ground such as incoming Japan, South Korea, Vietnam, are one afterwards The time-honored traditional medicine of kind.Green plum is rich in organic acid abundant, carbohydrate, amino acid, volatile component and flavonoids, cyanine The phenolic substancess such as element have antibacterial, anticancer, anti-oxidant, anti-inflammatory and other effects.Existing green plum class product has in the market: green plum Preserved fruit, dried fruit, jam, dark-plum juice drink, green liquor etc., this kind of leisure product is concerned only with the flavor of green plum, in the form of a single, suddenly Depending on its important drug effect value, economic value is low.Therefore, the exploitation health-related product of green plum is by the pattern of abundant green plum product, And effectively improve the economic value of green plum.
The price of green plum is relatively low, and annual yield is huge, meanwhile, the raw material compared to most of integration of drinking and medicinal herbs is deposited Poor taste, Chinese medicine is highly seasoned the disadvantages of, the refreshing taste of green plum acid, strong fruity are easier to that people is allowed to receive.Therefore, it is necessary to develop Green plum oral spray class product improves the economic value of green plum to reduce the cost of spray.
Summary of the invention
The purpose of the present invention is to provide a kind of green plum oral spray and preparation method thereof, have spray good effect, The wide advantage at low cost, in good taste of raw material sources.
The technical solution adopted by the present invention is that:
A kind of green plum oral spray, is made of the raw material of following mass fraction: 5-10 parts of green plum polyphenol, permeation enhancers 1- 8 parts, 1-5 parts of sweetener, 0-1 parts of preservative, 76-90 parts of water.
Further, green plum oral spray as described above, is made of the raw material of following mass fraction: 8 parts of green plum polyphenol, 5 parts of permeation enhancers, 3 parts of sweetener, 0.04 part of preservative, 80 parts of water.
Further, green plum oral spray as described above, the permeation enhancers are polyethylene glycol, glycerol, propylene glycol, gallbladder The mixture of one or more of hydrochlorate.
Further, green plum oral spray as described above, the sweetener be one of xylitol, antierythrite or Two kinds.
A kind of preparation method of green plum oral spray, comprising the following steps:
(1) extract green plum polyphenol: green plum is dry, crushing, sieving, solubilizer extract to obtain green plum polyphenol extract liquor, later Extract liquor is concentrated to give green plum polyphenol;
(2) the green plum polyphenol extract liquor of concentration is dissolved in the water with permeation enhancers, sweetener, is stirred, after being completely dissolved Packing, sterilizing.
Further, the dry method of the green plum are as follows: fresh, mature green plum is selected, cleans, stoning, cuts in half, Under the conditions of -45 DEG C, 10Pa, vacuum freeze drying 48h.
Further, the crushing, sieving, extraction process of step (1) are as follows: the green plum after drying is pulverized, excessively 100~ 80% ethyl alcohol of 10~15 times of mass ratioes is added in 200 meshes, extracts 10~30min, filters to obtain green plum polyphenol extract liquor, described Extracting method is 300~500W ultrasonic extraction or 300~500W ultrasonic extraction or 500~600MPa superelevation under ice bath state It is extracted under the conditions of pressure.
Further, when extraction, addition and ascorbic acid of the solvent volume than 1%~3%.
Further, the method for concentration of the green plum polyphenol extract liquor are as follows: by extract liquor at -15 DEG C freeze concentration 1.5h。
Further, the sterilising conditions are ultra-high pressure sterilization 20min under 500MPa.
The beneficial effects of the present invention are:
A kind of green plum oral spray is made in green plum by the present invention, due to being rich in phenolic substances and organic acid in green plum, no Only flavor faint scent, moreover it is possible to inhibit the growth of streptococcus mutans, carry out effective antibacterial, fresh breath can be reached and played anti- The effect of saprodontia overcomes the deficiency that existing oral spray curative effect is general, effect is single;The available of green plum is increased simultaneously Approach has widened the market of green plum, increases the pattern of oral spray.
Xylitol, the antierythrite used, referred to as zero calorific value ingredient, taste is similar to sucrose, can as sweetener into Row seasoning, and calorific value is close to zero;Meanwhile the streptococcus mutans in oral cavity cannot utilize and ferment xylitol or red used The sugar alcohols such as moss sugar alcohol lead to saprodontia so the decline of dental surface pH value will not be caused to generate dental plaque.
Compared to traditional solvent extraction active constituent, ultrasonic extraction of the invention has great advantage, and ultrasonic wave is in matchmaker When propagating in matter, by mechanism, cavitation and heat effect, the series of effects such as mechanics, calorifics, optics, chemistry are generated, Accelerate the destruction of raw material cell wall, improves solvent penetration speed, be dissolved into green plum polyphenol in solvent rapidly, improve extraction Rate, while shortening extraction time.
Using vacuum refrigeration concentration technique, it is performed under reduced pressure freeze concentration, the boiling point of feed liquid can be reduced, is shortened dense The contracting time utmostly reduces polyphenol oxidase under conditions of preventing oxygen and participating in and decomposes.
Specific embodiment
Below with reference to embodiment, the present invention will be further described.
Embodiment 1
A kind of green plum oral spray, is made of the raw material of following quality: green plum polyphenol 8g, polyethylene glycol 5g, xylitol 3g, potassium sorbate 0.04g, water 84g.
Preparation method are as follows:
(1) the fresh green plum that pulp is full, fruit stone is small is chosen, removal of impurities, is cleaned stalk, is drained away the water, is gone with corer After core, pulp cut in half, 100g pulp pre-freeze 5h (- 75 DEG C) in ultra low temperature freezer are weighed;
(2) vacuum freeze drying: -45 DEG C, 10Pa vacuum freeze drying 48h is carried out after Green plum flesh pre-freeze, then with height Fast pulverizer carries out coarse crushing and obtains green plum coarse powder, pulverizes green plum coarse powder by ball milling instrument, crosses 160 meshes, it is unsifted again Secondary ball milling, until whole green plum coarse powder pulverized 160 meshes;
(3) 80% ethyl alcohol of 1L is added in green plum Ultramicro-powder, after stirring and evenly mixing, 500W ultrasonic extraction 20min is filtered Green plum polyphenol extract liquor;
(4) 1.5h is concentrated in -15 DEG C of vacuum refrigerations in green plum polyphenol extract liquor, obtains green plum polyphenol;
(5) 8g green plum polyphenol and 5g polyethylene glycol, 3g xylitol are dissolved in 84g water, stir, is dispensed after being completely dissolved At mono- bottle of 25mL, 500MPa ultra-high pressure sterilization 20min.
Embodiment 2
The present embodiment the difference from embodiment 1 is that: replace polyethylene glycol with glycerol or propylene glycol or cholate.
Embodiment 3
The present embodiment and the difference of embodiment 1,2 are: replacing xylitol with antierythrite.
Embodiment 4
The present embodiment and the difference of embodiment 1,2,3 are: ultrasonic extraction green plum polyphenol be under ice bath state and is carried out, It is characterized in that low temperature can inhibit the activity of polyphenol oxidase in extraction process, the loss of green plum polyphenol can be reduced.With room temperature Under the conditions of extract and compare, fungistatic effect increases 80-120%.
Embodiment 5
The present embodiment and the difference of embodiment 1,2,3 are: green plum polyphenol extracting method uses ultra high pressure extraction: 500MPa Ultra high pressure extraction 30min filters to obtain green plum polyphenol extract liquor, it is characterized in that in extraction process room temperature or lower than in room temperature into Row, can reduce the loss of green plum polyphenol.Compared with extracting under household condition, fungistatic effect increases 80-120%.
Embodiment 6
The present embodiment and the difference of embodiment 1,2,3 are: use microwave abstracting green plum polyphenol: after green plum is beaten, Microwave power 500W, 50 DEG C extract 5~10min with 55% ethyl alcohol, filter to obtain green plum extract liquor.With extract under household condition It compares, fungistatic effect increases 80-120%.
Embodiment 7
The present embodiment and the difference of embodiment 1,2,3 are: 2g ascorbic acid is added in green plum Ultramicro-powder, pours into 1L 80% ethyl alcohol carries out the extraction of green plum polyphenol after stirring and evenly mixing.Compared with extracting under household condition, fungistatic effect increases 80- 120%.
Embodiment 8
The antibacterial experiment in vitro report of green plum oral spray of the present invention illustrates its effect:
Main pathogenic bacteria-of the obtained green plum oral spray of 1~7 method of Application Example difference to dental decayed tooth Streptococcus mutans (ATCC 25175) have carried out paper disk method and constant dilution method bacteriostatic experiment, are as a result reported as follows:
One, paper disk method
1, culture medium, condition of culture, operating method are identical as constant dilution method.
2, routinely operating method makes the antibacterial scraps of paper, soaks paper with 7 kinds of green plum oral sprays of concentration 1g/ml respectively Piece, scraps of paper ultimate density are (10ul/ piece).
3, the brain-heart infusion medium (BHI) of Fresh is inoculated with above-mentioned thin in advance by above-mentioned bacteria resuscitation culture 48h Bacterium is applied on plate respectively, places above-mentioned 7 kinds of antibacterial scraps of paper respectively, and Anaerobic culturel 48h takes out, without bacterial growth around measurement Most short diameter is the antibacterial ring size of the oral spray.
The above experiment in triplicate, the results are shown in Table 1.
Antibacterial table (mm) of the 17 kinds of preparation method green plum oral sprays of table to streptococcus mutans
As seen from Table 1,7 kinds of green plum oral sprays have fungistatic effect to streptococcus mutans, and average inhibition zone range exists 4.00~15.00mm.
Two, constant dilution method
(1) 7 kinds of different resulting green plum oral sprays of preparation method are distinguished into two-fold dilution to 8 by constant dilution method is conventional It manages, mixture total volume is 2mL in every pipe, and antimicrobial concentration successively successively decreases respectively, and whole green plum oral spray concentration is respectively 320、160、80、40、20、10、5、2.5、1.25ug/mL。
(2) it prepares BHI solid medium to be put into flask, sterilize, be cooled to 40 DEG C or so for use.
(3) the green plum oral spray of various concentration in (1) is added different equipped with sterilized BHI solid medium Flask in, make the volume 1:9 of solution and culture medium.
(4) it is poured into after mixing well in the sterile glass plate that diameter is 90mm, 37 DEG C of constant temperature trainings of anaerobic environment Support 48h.
(5) bacterium colony growing state is observed, is minimum antibacterial dense with sterile contained lowest concentration of drug in long plate of being born It spends (MIC).
Experiment is repeated 3 times, and the results are shown in Table 2.
Inhibition situation of the 27 kinds of preparation method green plum oral sprays of table to streptococcus mutans
Note: 1. "+" indicates bacterium colony growth;2. "-" indicates sterile length of being born.
Above-mentioned laboratory report shows 7 kinds of different resulting green plum oral sprays of preparation method to the minimum of streptococcus mutans Bacteriocidal concentration MIC (ug/ml) value range is 40~80.
Embodiment 9
The present embodiment and the difference of embodiment 8 be, antibacterial experiment in vitro two, in the premise for giving sufficient culture medium Under, do not limit its culture period, as a result, it has been found that, 7 kinds of preparation method green plum oral sprays to the inhibitory effects of streptococcus mutans at any time Increase and weaken until disappear, antibacterial time range value be 48~72h.

Claims (10)

1. a kind of green plum oral spray, which is characterized in that be made of the raw material of following mass fraction: 5-10 parts of green plum polyphenol, 1-8 parts of permeation enhancers, 1-5 parts of sweetener, 0-1 parts of preservative, 76-90 parts of water.
2. a kind of green plum oral spray as described in claim 1, which is characterized in that by the raw material group of following mass fraction At: 8 parts of green plum polyphenol, 5 parts of permeation enhancers, 3 parts of sweetener, 0.04 part of preservative, 80 parts of water.
3. a kind of green plum oral spray as described in claim 1, which is characterized in that the permeation enhancers be polyethylene glycol, The mixture of one or more of glycerol, propylene glycol, cholate.
4. a kind of green plum oral spray as described in claim 1, which is characterized in that the sweetener is xylitol, red moss One or both of sugar alcohol.
5. the preparation method of any green plum oral spray as described in Claims 1 to 4, which is characterized in that including with Lower step:
(1) extract green plum polyphenol: green plum is dry, crushing, sieving, solubilizer extract to obtain green plum polyphenol extract liquor, later will extraction Liquid is taken to be concentrated to give green plum polyphenol;
(2) the green plum polyphenol extract liquor of concentration is dissolved in the water with permeation enhancers, sweetener, is stirred, dispensed after being completely dissolved, Sterilizing.
6. a kind of preparation method of green plum oral spray as claimed in claim 5, which is characterized in that the green plum drying Method are as follows: fresh, mature green plum is selected, cleans, stoning, cuts in half, under the conditions of -45 DEG C, 10Pa, vacuum freeze drying 48h。
7. a kind of preparation method of green plum oral spray as claimed in claim 5, which is characterized in that the crushing of step (1), Sieving, extraction process are as follows: the green plum after drying is pulverized, 100~200 meshes are crossed, 10~15 times of mass ratioes are added 80% ethyl alcohol extracts 10~30min, filters to obtain green plum polyphenol extract liquor, the extracting method be 300~500W ultrasonic extraction or It is extracted under 300~500W ultrasonic extraction or 500~600MPa ultra-high pressure condition under ice bath state.
8. a kind of preparation method of green plum oral spray as claimed in claim 5, which is characterized in that when extraction, addition with Ascorbic acid of the solvent volume than 1%~3%.
9. a kind of preparation method of green plum oral spray as claimed in claim 5, which is characterized in that the green plum polyphenol extraction Take the method for concentration of liquid are as follows: by extract liquor at -15 DEG C freeze concentration 1.5h.
10. a kind of preparation method of green plum oral spray as claimed in claim 5, which is characterized in that the sterilising conditions For ultra-high pressure sterilization 20min under 500MPa.
CN201811602647.6A 2018-12-26 2018-12-26 A kind of green plum oral spray and preparation method thereof Pending CN109568413A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN110123710A (en) * 2019-05-15 2019-08-16 西华大学 A kind of plum fruit bath salt and preparation method thereof, application

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CN101254224A (en) * 2008-02-26 2008-09-03 陈光英 Green prune extract of anti acquired immuno-deficiency syndrome and bacterium

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110123710A (en) * 2019-05-15 2019-08-16 西华大学 A kind of plum fruit bath salt and preparation method thereof, application

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