CN108852953A - A kind of formula and technique of Xinhui citrus reticulata unshiu peel extract production toothpaste - Google Patents
A kind of formula and technique of Xinhui citrus reticulata unshiu peel extract production toothpaste Download PDFInfo
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Abstract
The invention discloses a kind of formulas of Xinhui citrus reticulata unshiu peel extract production toothpaste, and it includes the components of following mass percent：The moisturizer of 40.0-60.0%, the rubbing agent of 15.0-25.0%, the Xinhui citrus reticulata unshiu peel extract of 10.0-15.0%, the surfactant of 1.0-3.0%, the thickener of 1.0-2.0%, the essence of 0.8-1.4%, the sweetener of 0.1-0.2%, the preservative of 0.1-0.2% and suitable deionized water.The invention also discloses a kind of techniques of Xinhui citrus reticulata unshiu peel extract production toothpaste.For the present invention, Xinhui citrus reticulata pericarp is extracted using carbon dioxide supercritical extraction technology, and by optimal Xinhui citrus reticulata unshiu peel extract content combination food grade accessories, in addition to having and cleaning one's teeth and protect tooth, go the basic function of removing abnormal flavor in oral cavity and stain dirt, the growth of Buccodental harmful bacteria, bactericidal antiphlogistic and other effects can also effectively be inhibited, the symptoms such as tooth swelling, bleeding, pain caused by capable of being effectively relieved because of gingivitis, periodontitis, canker sore have significant prevention and remission effect to common oral disease.
Description
Technical field
The invention belongs to oral care implement technical fields, and in particular to a kind of Xinhui citrus reticulata unshiu peel extract production toothpaste
Formula and technique.
Background technique
Xinhui citrus reticulata, the also known as wide old mandarin orange of newly meeting or dried orange peel mandarin orange, the famous local and special products in Jiangmen City of Guangdong Province Xinhui District, Chinese geography mark
Will product.Xinhui citrus reticulata, skin and flesh dual-purpose, integration of drinking and medicinal herbs is wide old mandarin orange agriculture in very long plantation history, bright red from Rutaceae Citrus
The outstanding kind screened in mandarin orange.Its quality is unique, is just in fashion various regions in Ming and Qing, and be listed in " tribute ", pays a tribute year after year.
Orange peel is the most important byproduct remained after citrusfruit is processed, and contained nutritional ingredient removes amino acid
Outside, remaining is above pulp, is especially enriched in certain function ingredient, as flavonoids, limonoid, carotenoid, phenolic acid,
The substances such as pectin and dietary fiber.These substances have many physiological activity such as anticancer, anti-oxidant, antibacterial, have to human health
There is important health-care effect.Wherein, the Flavonoid Content in mandarin orange pericarp is especially abundant, and content is much higher than fruit juice.
Flavonoids is a kind of with C6-C3-C6Benzene-gamma-pyrone structure polyphenol compound, is chromone or chromogen
The derivative of alkane.Currently, separation identifies 60 various of monomer flavone compounds from citrus plant, it is broadly divided into three
Class：Flavanones (including 3- hydroxyl flavanones or dihydro flavanones), flavones (including 3-hydroxyflavone or flavonols) and anthocyanin.
Flavonoids is considered as one of most important effective component in citrus, has and maintains blood vessel normal osmotic pressure, enhancing capillary
Toughness shortens the bleeding time, reduces cholesterol, antiallergy, antiviral, anti-inflammatory, inhibits the effects of cancer cell growth and transfer.
In the prior art, once saw that the natural materials such as Camellia nitidissima, mother chrysanthemum tea, green tea, small algae ball, Pu'er tea were used in toothpaste
For preventing the report of mouth disease, but have no the relevant report being applied to Xinhui citrus reticulata unshiu peel extract in toothpaste.
Summary of the invention
In order to overcome the above technical defects, there is provided a kind of Xinhui citrus reticulata unshiu peel extracts to make for the first object of the present invention
The formula of toothpaste, the Xinhui citrus reticulata unshiu peel extract extracted containing method provided by the present invention and food grade accessories,
In addition to having and cleaning one's teeth and protect tooth, go the basic function of removing abnormal flavor in oral cavity and stain dirt, additionally it is possible to effectively inhibition Buccodental harmful bacteria
Growth, bactericidal antiphlogistic and other effects.
To solve the above-mentioned problems, the present invention is achieved by following technical scheme：
A kind of formula of Xinhui citrus reticulata unshiu peel extract production toothpaste, the component comprising following mass percent：
Further, the component comprising following mass percent：
Further, the Xinhui citrus reticulata unshiu peel extract uses carbon dioxide supercritical extraction technology.
Further, the preparation method of the Xinhui citrus reticulata unshiu peel extract is：
1) fresh Xinhui citrus reticulata pericarp is cut into thin strips shape, in 50-60 DEG C of heated-air drying, grinds, sieving；
2) entrainer is added, carbon dioxide supercritical extraction, extraction are carried out to Xinhui citrus reticulata pericarp powder obtained by step 1)
Take temperature be 40-60 DEG C, extracting pressure 200-500BAR, extraction time 1-3h, using after reduced pressure to get described
Xinhui citrus reticulata unshiu peel extract.
When temperature is lower than 50 DEG C, after extracting flavonoids rate increases as the temperature rises, but temperature is higher than 50 DEG C, flavones
Recovery rate is reduced instead, this is because extraction temperature has dual influence to effect of extracting.On the one hand, temperature raising is conducive to
The diffusion coefficient of solute volatile increase and raising material, the extraction for being conducive to flavone compound in mandarin orange pericarp go out；Another party
Face, temperature increase the concentration for reducing carbon dioxide again, reduce the density of carbon dioxide, so as to cause carbon dioxide solubility energy
The reduction of power is unfavorable for extracting.In addition, temperature increases the physiological activity that can also destroy the flavone compound of extraction.Therefore, extract
The temperature taken is unsuitable excessively high.
The increase of pressure increases the density of supercritical carbon dioxide fluid, is conducive to the dissolution of flavones ingredient, but
It is that the diffusion coefficient of supercritical carbon dioxide fluid also reduces with the increase of pressure, and is unfavorable for the dissolution of flavones ingredient；
When pressure is in 200-300BAR, recovery rate rises with pressure and is increased, and since 300BAR, recovery rate with pressure rising
And it reduces.Therefore, the pressure of extraction is unsuitable excessively high.
The molecular structure of carbon dioxide determines that it has certain limitation to certain separation process：For hydro carbons and weak
The solvability of polar liposoluble substance is preferable, but highly polar organic compound is then needed to increase extracting pressure or use
Entrainer separates to realize.Carbon dioxide is apolar substance, simple supercritical carbon dioxide fluid can only extract polarity compared with
Low lipophilic substance, the general polarity of Flavonoid substances is larger, can only obtain under conditions of entrainer is not added a small amount of volatile
Small-molecule substance, the yield of flavone compound is extremely low, and therefore, it is necessary to improve flavone compound by the way that entrainer is added
Recovery rate.
Further, in step 2), the entrainer is 70% ethyl alcohol, 95% ethyl alcohol, dehydrated alcohol or methanol；It is preferred that
, the entrainer is methanol.
When selecting entrainer, 70% ethyl alcohol, 95% ethyl alcohol and dehydrated alcohol are chosen, due in organic solvent, methanol
Polarity is greater than ethyl alcohol, and the boiling point of methanol is than the low boiling point of dehydrated alcohol.Therefore, selection methanol may be more advantageous to flavones
The extraction and separation of class compound.
It further, is first 1 by solid-liquid ratio g/mL in step 2):The entrainer, static extracting is added in (0.5-2)
20min, then the entrainer, dynamic extraction 2h are added by 0.2-0.6mL/min；Preferably, first pressing solid-liquid ratio is 1:1 is added institute
Entrainer, static extracting 20min are stated, then adds the entrainer, dynamic extraction 2h by 0.4mL/min.
When dynamic extraction, when entrainer additional amount is 0.4mL/min or so, recovery rate highest.With entrainer dosage
Increase, is conducive to the dissolution of the flavone compound in mandarin orange pericarp, increases recovery rate；But dosage is excessive, in mandarin orange pericarp
The time of contact of flavone compound and entrainer shortens, and leads to the reduction of entrainer service efficiency.
When dynamic extraction, the time is longer, and the recovery rate of flavone compound is higher.But after 120min, general flavone leaching content
Seldom, this is because under normal circumstances, if extraction time is too short, supercritical carbon dioxide fluid not up to well connects with solute
Touching, extraction quantity are few；After a certain period of time, supercritical fluid and flavone compound move closer to dissolution equilibrium for extraction, are further added by extraction
The time is taken, extraction yield increase is limited, and with the extension of time, the energy consumption of supercritical extract is also increasing.
Further, the general flavone content of the Xinhui citrus reticulata unshiu peel extract is greater than 10%.
Further, the moisturizer is at least one of glycerol, sorbierite, polyethylene glycol, propylene glycol；The friction
Agent is at least one of calcium carbonate, calcium monohydrogen phosphate, calcium pyrophosphate, silica, aluminium hydroxide；The surfactant is ten
At least one of glycol sodium sulphate, 2- acyloxy key sodium sulfonate；The thickener is carboxymethyl cellulose, carboxyethylcellulose
At least one of element, deer horn pectin, xanthan gum, guar gum；The sweetener is xylitol or saccharin sodium；The preservative is
Sorbic acid sylvite or sodium benzoate；The fragrance is menthol or fruits fragrance.
Further, the moisturizer is glycerol and sorbierite；The rubbing agent is silica；The surfactant
For sodium lauryl sulfate；The thickener is carboxymethyl cellulose and xanthan gum；The sweetener is xylitol；The preservative
For sodium benzoate；The fragrance is menthol.
It selects glycerol and sorbierite as moisturizer, toothpaste cure hard in hose can be prevented, and make lotion that there is light
The efficiency such as pool；It selects silica as rubbing agent, has and buy strong tooth ability, good physical performance, chemical property stabilization and toothpaste
The good advantage of the compatibility of other ingredients in lotion, moreover, the specific surface of silica is big, it is strong to the adsorption capacity of fragrance, make
The fragrance of toothpaste becomes soft and persistently improves lotion glossiness, and mouthfeel is more fine and smooth；Carboxymethyl cellulose and xanthan gum is selected to make
For thickener, it can improve and increase the viscosity of lotion, keep the stability of lotion, and improve the physical behavior of lotion,
And make the mouthfeel of toothpaste more preferably；Select xylitol as sweetener, with high security, cause the sense of taste is good, stability is high,
The advantages that good water solubility, and reasonable price；It selects sodium benzoate as preservative, microorganism growth can be postponed or chemistry becomes
Corruption caused by changing, the more conducively effective component in holding toothpaste；Select menthol as fragrance, so that toothpaste has mint flavored
Faint scent, cool taste.
In order to overcome the above technical defects, there is provided a kind of Xinhui citrus reticulata unshiu peel extracts to make for the second object of the present invention
The process of toothpaste, this method prepare simple and fast.
To solve the above-mentioned problems, the present invention is achieved by following technical scheme：
A kind of process of Xinhui citrus reticulata unshiu peel extract production toothpaste, includes the following steps：
S1, ingredient：It is equipped with the raw material components comprising following mass percent：The moisturizer of 40.0-60.0%, 15.0-
25.0% rubbing agent, the Xinhui citrus reticulata unshiu peel extract of 10.0-15.0%, the surfactant of 1.0-3.0%, 1.0-2.0%
Thickener, the essence of 0.8-1.4%, the sweetener of 0.1-0.2%, 0.1-0.2% preservative and suitable deionization
Water；
S2, the appropriate deionized water is added in Xinhui citrus reticulata unshiu peel extract provisioned in step S1, adds step
Thickener provisioned in rapid S1 stands after dissolve after its swelling completely, is added in toothpaste Manufacturing medicine extract machine；
S3, by the moisturizer, the sweetener provisioned in step S1, the preservative and the remaining deionized water
Stirring and dissolving is then added in toothpaste Manufacturing medicine extract machine described in step S2, and the toothpaste Manufacturing medicine extract machine is stirred at low speed and vacuumized, to true
Reciprocal of duty cycle closes vacuum pump when reaching -0.09MPa；
S4, make toothpaste Manufacturing medicine extract machine high-speed stirred described in step S3, by the rubbing agent, the table provisioned in step S1
Face activating agent is successively drawn into the toothpaste Manufacturing medicine extract machine using the vacuum pump, opens the vacuum pump, hybird environment it is true
Reciprocal of duty cycle continues 20~30min of homogeneous when reaching -0.09~-0.095MPa, and lotion is made to reach tight, is then shut off described true
Sky pump, essence provisioned in step S1 is drawn into the toothpaste Manufacturing medicine extract machine by the vacuum pump；
S5, the vacuum pump continuation 10~20min of homogeneous is opened, obtains with certain viscosity, dilute thick lotion appropriate,
Filling, packaging is carried out after quality inspection is qualified, can be prepared by required toothpaste finished product.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) formula of a kind of Xinhui citrus reticulata unshiu peel extract production toothpaste provided by the invention, using CO 2 supercritical
Abstraction technique extracts Xinhui citrus reticulata pericarp, and the general flavone content of extract liquor is greater than 10%, and the flavone compound is to gold
Staphylococcus aureus, hemolytic streptococcus, lactobacillus, anaerobism, which expand bacterium, lactobacillus acidophilus, Escherichia coli, has different degrees of suppression
System, can be used as a kind of natural antibacterial active material；By the optimum content and food grade accessories of choosing Xinhui citrus reticulata unshiu peel extract
In conjunction in addition to having and cleaning one's teeth and protect tooth, go the basic function of removing abnormal flavor in oral cavity and stain dirt, additionally it is possible to effectively inhibit Buccodental nocuousness
Bacteria breed, bactericidal antiphlogistic and other effects, tooth swelling caused by capable of being effectively relieved because of gingivitis, periodontitis, canker sore go out
The symptoms such as blood, pain have significant prevention and remission effect to common oral disease.
(2) process of Xinhui citrus reticulata unshiu peel extract production toothpaste of the present invention, this method prepares simple and efficient.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing, wherein：
Fig. 1 is the process flow chart that Xinhui citrus reticulata unshiu peel extract of the present invention makes toothpaste.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
The invention discloses a kind of formula of Xinhui citrus reticulata unshiu peel extract production toothpaste, the group comprising following mass percent
Point：
Wherein, moisturizer is at least one of glycerol, sorbierite, polyethylene glycol, propylene glycol；Rubbing agent be calcium carbonate,
At least one of calcium monohydrogen phosphate, calcium pyrophosphate, silica, aluminium hydroxide；Surfactant is sodium lauryl sulfate, 2- acyl
At least one of oxygroup key sodium sulfonate；Thickener is carboxymethyl cellulose, carboxyethyl cellulose, deer horn pectin, xanthan gum, melon
At least one of your glue；Sweetener is xylitol or saccharin sodium；Preservative is sorbic acid sylvite or sodium benzoate；Fragrance is thin
Lotus alcohol or fruits fragrance.
Various test apparatuses and reagent are commercial goods, are that can buy to obtain by commercial sources.
Embodiment 1
(1) preparation of Xinhui citrus reticulata unshiu peel extract：
1) fresh Xinhui citrus reticulata pericarp is cut into thin strips shape, in 55 DEG C of heated-air dryings, grinds, sieving；
2) it takes out 100g dry powder and 100mL methanol is added, be 50 DEG C in extraction temperature, extracting pressure is the condition of 300BAR
Under, static extracting 20min, then by 0.4mL/min add methanol, dynamic extraction 2h, using after reduced pressure to get 22.2g
Xinhui citrus reticulata unshiu peel extract.
(2) a kind of formula of Xinhui citrus reticulata unshiu peel extract production toothpaste, the component comprising following quality：
(3) process of Xinhui citrus reticulata unshiu peel extract production toothpaste, includes the following steps：
S1, ingredient：It is equipped with the raw material components comprising following mass percent：The glycerol of 25.0g, 25.0g sorbierite,
The silica of 20.0g, the Xinhui citrus reticulata unshiu peel extract of 12.0g, the sodium lauryl sulfate of 2.0g, 0.75g carboxymethyl cellulose
The deionization of element, the xanthan gum of 0.75g, the menthol of 1.0g, the xylitol of 0.15g, the sodium benzoate of 0.15g and 13.2g
Water；
S2, appropriate amount of deionized water is added in Xinhui citrus reticulata unshiu peel extract provisioned in step S1, adds step S1 and is matched
Standby carboxymethyl cellulose, xanthan gum stand after dissolve after its swelling completely, are added in toothpaste Manufacturing medicine extract machine；
S3, by glycerol provisioned in step S1, sorbierite, xylitol, sodium benzoate and remaining deionized water stirring and dissolving,
It is then added in the toothpaste Manufacturing medicine extract machine of step S2, toothpaste Manufacturing medicine extract machine is stirred at low speed and vacuumized, and reaches -0.09MPa to vacuum degree
When close vacuum pump；
S4, the toothpaste Manufacturing medicine extract machine high-speed stirred for making step S3, by silica provisioned in step S1, sodium lauryl sulfate
Successively be drawn into toothpaste Manufacturing medicine extract machine using vacuum pump, open vacuum pump, when the vacuum degree of hybird environment reaches -0.095MPa after
Continuous homogeneous 25min, makes lotion reach tight, is then shut off vacuum pump, menthol provisioned in step S1 is passed through vacuum
Pump is drawn into toothpaste Manufacturing medicine extract machine；
S5, vacuum pump continuation homogeneous 15min is opened, obtains with certain viscosity, dilute thick lotion appropriate, is examined through quality
Filling, packaging is carried out after testing qualification, can be prepared by required toothpaste finished product.
Embodiment 2
(1) preparation of Xinhui citrus reticulata unshiu peel extract：
1) fresh Xinhui citrus reticulata pericarp is cut into thin strips shape, in 50 DEG C of heated-air dryings, grinds, sieving；
2) it takes out 100g dry powder and 50mL methanol is added, be 40 DEG C in extraction temperature, under conditions of extracting pressure is 200BAR,
Static extracting 20min, then methanol is added by 0.2mL/min, dynamic extraction 2h newly can using after reduced pressure to get 20.1g
Mandarin orange unshiu peel extract.
(2) a kind of formula of Xinhui citrus reticulata unshiu peel extract production toothpaste, the component comprising following quality：
(3) process of Xinhui citrus reticulata unshiu peel extract production toothpaste is same as Example 1.
Embodiment 3
(1) preparation of Xinhui citrus reticulata unshiu peel extract：
1) fresh Xinhui citrus reticulata pericarp is cut into thin strips shape, in 60 DEG C of heated-air dryings, grinds, sieving；
2) it takes out 100g dry powder and 200mL methanol is added, be 60 DEG C in extraction temperature, extracting pressure is the condition of 500BAR
Under, static extracting 20min, then by 0.6mL/min add methanol, dynamic extraction 2h, using after reduced pressure to get 21.3g
Xinhui citrus reticulata unshiu peel extract.
(2) a kind of formula of Xinhui citrus reticulata unshiu peel extract production toothpaste, the component comprising following quality：
(3) process of Xinhui citrus reticulata unshiu peel extract production toothpaste is same as Example 1.
Embodiment 4
(1) preparation method of Xinhui citrus reticulata unshiu peel extract is same as Example 1.
(2) a kind of formula of Xinhui citrus reticulata unshiu peel extract production toothpaste, the component comprising following quality：
(3) process of Xinhui citrus reticulata unshiu peel extract production toothpaste, includes the following steps：
S1, ingredient：It is equipped with the raw material components comprising following mass percent：The third the two of the polyethylene glycol of 25.0g, 25.0g
The carboxylic second of alcohol, the aluminium hydroxide of 20.0g, the Xinhui citrus reticulata unshiu peel extract of 12.0g, the 2- acyloxy key sodium sulfonate of 2.0g, 0.75g
Base cellulose, the guar gum of 0.75g, the Orange flavor essence of 1.0g, the saccharin sodium of 0.15g, 0.15g sorbic acid sylvite and
13.2g deionized water；
S2, appropriate amount of deionized water is added in Xinhui citrus reticulata unshiu peel extract provisioned in step S1, adds step S1 and is matched
Standby carboxyethyl cellulose, guar gum stand after dissolve after its swelling completely, are added in toothpaste Manufacturing medicine extract machine；
S3, polyethylene glycol provisioned in step S1, propylene glycol, saccharin sodium, sorbic acid sylvite and remaining deionized water are stirred
Dissolution to be mixed, is then added in the toothpaste Manufacturing medicine extract machine of step S2, toothpaste Manufacturing medicine extract machine is stirred at low speed and is vacuumized, reach to vacuum degree-
Vacuum pump is closed when 0.09MPa；
S4, the toothpaste Manufacturing medicine extract machine high-speed stirred for making step S3, by aluminium hydroxide provisioned in step S1,2- acyloxy key sulphur
Sour sodium is successively drawn into toothpaste Manufacturing medicine extract machine using vacuum pump, and vacuum pump is opened, and the vacuum degree of hybird environment reaches -0.095MPa
Shi Jixu homogeneous 20min, makes lotion reach tight, is then shut off vacuum pump, by Orange flavor essence provisioned in step S1
It is drawn into toothpaste Manufacturing medicine extract machine by vacuum pump；
S5, vacuum pump continuation homogeneous 10min is opened, obtains with certain viscosity, dilute thick lotion appropriate, is examined through quality
Filling, packaging is carried out after testing qualification, can be prepared by required toothpaste finished product.
Physical and chemical index and Stability Determination
Toothpaste obtained by embodiment 1-4 is subjected to physical and chemical index and Stability Determination, test result are as shown in table 1.
1 physical and chemical index of table and Stability Determination result
As shown in Table 1, toothpaste indices obtained by the embodiment of the present invention 1-4 meet national standard (GB8372-
2017 and QB2966-2014).
Effete test embodiment 1
Newly the antibacterial effect of flavonoids is tested in meeting unshiu peel extract：
(1) prepared by strains tested suspension：6 kinds are inoculated in solid broth bouillon respectively for examination strain, in 37 DEG C
Constant temperature incubation is for 24 hours；The fungus block that the media surface of strain inclined plane activation has been carried out with inoculation hook picking, is added sterile physiological salt
Water is ground uniformly in tissue grinder, and the concentration of bacteria suspension is adjusted to 1 × 106-6×106cfu/mL。
(2) bacteriostatic test：LB solid medium is prepared, solid medium fusing is poured into culture dish after cooling, solidification,
Dip the bacteria suspension of each test organisms respectively with sterile cotton swab, plate containing bacterium is made in even spread media surface.Using filter paper
Piece method, it is dry after high pressure sterilization is handled by the filter paper dick of diameter 5mm, 10 μ L, 10% 1-4 of embodiment of the present invention institute is added dropwise
DMSO liquid is added dropwise as negative control as test print in Xinhui citrus reticulata unshiu peel extract obtained, with aseptic nipper by test sample
Piece and negative control print are placed in each culture dish surface, cover culture dish, for 24 hours in 37 DEG C of cultures.Test result such as 2 institute of table
Show.
Antibacterial activity test result of the 2 Xinhui citrus reticulata unshiu peel extract of table to 6 kinds of tested bacterium
Note："—"：Without bacteriostatic activity；Antibacterial circle diameter：In terms of mm.
As shown in Table 2, Xinhui citrus reticulata unshiu peel extract obtained by the embodiment of the present invention 1-4 to staphylococcus aureus,
Hemolytic streptococcus, lactobacillus, anaerobism, which expand bacterium, lactobacillus acidophilus, Escherichia coli, has different degrees of inhibiting effect.
Effete test embodiment 2
Ordinary toothpaste using toothpaste obtained by the embodiment of the present invention 1-4 and on the market is (without activity of the invention
Ingredient) carry out clinical trial.It is specific as follows：
(1) according to the standard of clinical diagnosis canker sore, it is selected into 100 patients altogether, is divided into 5 experimental groups, every group 20.
Each group needs to have no significant difference (P > 0.05) in terms of age, gender, kinds of Diseases and ulcer, has comparable
Property；Wherein, canker sore 1 grade 5, canker sore 2 grades 5, canker sore 3 grades 5, canker sore 4 grades 5 in every group.
Canker sore classification：
1 grade：Callous ulcer, erythema or mild pain, are not required to anodyne；
2 grades：Pain need to use analgesic with erythema, oedema or dotted ulcer, moderate pain, but patient can consuming solid food
Object；
3 grades：Pain need to use stronger analgesic with erythema, oedema or sheet ulcer, and patient is unable to consuming solid foods, shadow
Ring rest；
4 grades：Mucous membrane ulcer, severe pain cannot be fed, and need parenteral or EN support.
(2) experimental method：
5 groups of canker sore patients select toothpaste made from toothpaste made from embodiment 1, embodiment 2, embodiment 3 to make respectively
Toothpaste, toothpaste made from embodiment 4, control group ordinary toothpaste (without active constituent of the invention) on the market carry out
It brushes teeth, once in the morning and once at night, persistently uses 3 months, without extra process, different time points carry out canker sore after choosing treatment
The detection that incidence detection and canker sore are classified.
(3) deliberated index：
A situation arises and ulcer size, depth, shape and surrounding mucosa register feelings for ulcer when detailed inspection treatment end
Condition.It is disappeared with canker sores and the healing of all ulcer wound surfaces is that index judges healing time.Test result is as shown in table 3.
3 different time canker sore of table healing number of cases situation
As shown in Table 3, toothpaste obtained by the embodiment of the present invention 1-4 has significant effect to treatment canker sore,
Its therapeutic effect is substantially better than reference examples.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, therefore
Without departing from the technical solutions of the present invention, according to the technical essence of the invention it is to the above embodiments it is any modification,
Equivalent variations and modification, all of which are still within the scope of the technical scheme of the invention.
Claims (10)
1. a kind of formula of Xinhui citrus reticulata unshiu peel extract production toothpaste, which is characterized in that the component comprising following mass percent：
2. the formula of Xinhui citrus reticulata unshiu peel extract production toothpaste according to claim 1, which is characterized in that include following matter
Measure the component of percentage：
3. the formula of Xinhui citrus reticulata unshiu peel extract production toothpaste according to claim 1, it is characterised in that：The Xinhui citrus reticulata
Unshiu peel extract uses carbon dioxide supercritical extraction technology.
4. the formula of Xinhui citrus reticulata unshiu peel extract production toothpaste according to claim 3, which is characterized in that the Xinhui citrus reticulata
The preparation method of unshiu peel extract is：
1) fresh Xinhui citrus reticulata pericarp is cut into thin strips shape, in 50-60 DEG C of heated-air drying, grinds, sieving；
2) entrainer is added, carbon dioxide supercritical extraction, extraction temperature are carried out to Xinhui citrus reticulata pericarp powder obtained by step 1)
Degree be 40-60 DEG C, extracting pressure 200-500BAR, extraction time 1-3h, using after reduced pressure to get the new meeting
Mandarin orange unshiu peel extract.
5. the formula of Xinhui citrus reticulata unshiu peel extract production toothpaste according to claim 4, it is characterised in that：In step 2)
In, the entrainer is 70% ethyl alcohol, 95% ethyl alcohol, dehydrated alcohol or methanol.
6. the formula of Xinhui citrus reticulata unshiu peel extract production toothpaste according to claim 4, it is characterised in that：In step 2)
In, it is first 1 by solid-liquid ratio g/mL:The entrainer, static extracting 20min is added in (0.5-2), then adds by 0.2-0.6mL/min
Add the entrainer, dynamic extraction 2h.
7. the formula of Xinhui citrus reticulata unshiu peel extract production toothpaste according to claim 4, it is characterised in that：The Xinhui citrus reticulata
The general flavone content of unshiu peel extract is greater than 10%.
8. the formula of Xinhui citrus reticulata unshiu peel extract production toothpaste according to claim 1, it is characterised in that：The moisturizer
For at least one of glycerol, sorbierite, polyethylene glycol, propylene glycol；The rubbing agent is calcium carbonate, calcium monohydrogen phosphate, pyrophosphoric acid
At least one of calcium, silica, aluminium hydroxide；The surfactant is sodium lauryl sulfate, 2- acyloxy key sulfonic acid
At least one of sodium；The thickener is carboxymethyl cellulose, in carboxyethyl cellulose, deer horn pectin, xanthan gum, guar gum
At least one；The sweetener is xylitol or saccharin sodium；The preservative is sorbic acid sylvite or sodium benzoate；The perfume (or spice)
Material is menthol or fruits fragrance.
9. the formula of Xinhui citrus reticulata unshiu peel extract production toothpaste according to claim 8, it is characterised in that：The moisturizer
For glycerol and sorbierite；The rubbing agent is silica；The surfactant is sodium lauryl sulfate；The thickener is
Carboxymethyl cellulose and xanthan gum；The sweetener is xylitol；The preservative is sodium benzoate；The fragrance is peppermint
Alcohol.
10. a kind of process of Xinhui citrus reticulata unshiu peel extract production toothpaste described in any item according to claim 1~9,
It is characterized in that, includes the following steps：
S1, ingredient：It is equipped with the raw material components comprising following mass percent：The moisturizer of 40.0-60.0%, 15.0-25.0%
Rubbing agent, the Xinhui citrus reticulata unshiu peel extract of 10.0-15.0%, the surfactant of 1.0-3.0%, 1.0-2.0% thickening
Agent, the essence of 0.8-1.4%, the sweetener of 0.1-0.2%, the preservative of 0.1-0.2% and suitable deionized water；
S2, the appropriate deionized water is added in Xinhui citrus reticulata unshiu peel extract provisioned in step S1, adds step S1
Provisioned thickener stands after dissolve after its swelling completely, is added in toothpaste Manufacturing medicine extract machine；
S3, the moisturizer, the sweetener provisioned in step S1, the preservative and the remaining deionized water are stirred
Dissolution, is then added in toothpaste Manufacturing medicine extract machine described in step S2, the toothpaste Manufacturing medicine extract machine is stirred at low speed and vacuumized, to vacuum degree
Vacuum pump is closed when reaching -0.09MPa；
S4, make toothpaste Manufacturing medicine extract machine high-speed stirred described in step S3, the rubbing agent provisioned in step S1, the surface is living
Property agent is successively drawn into the toothpaste Manufacturing medicine extract machine using the vacuum pump, and the vacuum pump, the vacuum degree of hybird environment are opened
Continue 20~30min of homogeneous when reaching -0.09~-0.095MPa, so that lotion is reached tight, be then shut off the vacuum
Pump, essence provisioned in step S1 is drawn into the toothpaste Manufacturing medicine extract machine by the vacuum pump；
S5, the vacuum pump continuation 10~20min of homogeneous is opened, with certain viscosity, dilute thick lotion appropriate is obtained, through matter
Amount carries out filling, packaging after the assay was approved, can be prepared by required toothpaste finished product.
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| CN201811139585.XA CN108852953A (en) | 2018-09-28 | 2018-09-28 | A kind of formula and technique of Xinhui citrus reticulata unshiu peel extract production toothpaste |
| PCT/CN2018/112368 WO2020062389A1 (en) | 2018-09-28 | 2018-10-29 | Formulation and process for preparing toothpaste from xinhui tangerine peel extract liquid |
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| CN101244016A (en) * | 2008-03-17 | 2008-08-20 | 柳州两面针股份有限公司 | Application of aurantiin in preparing oral cavity nursing health products |
| CN102579275A (en) * | 2012-02-22 | 2012-07-18 | 合肥学院 | Beautifying toothpaste containing aluminum-magnesium silicate and preparation method of beautifying toothpaste |
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| KR20090120833A (en) * | 2008-05-21 | 2009-11-25 | 한국생명공학연구원 | Extraction of neohesperidin from citrus peel by supercritical fluid extraction |
| CN103896898B (en) * | 2014-03-07 | 2016-04-20 | 中国计量科学研究院 | A kind of naringenin reference material and Synthesis and applications thereof |
| CN105147665A (en) * | 2015-09-16 | 2015-12-16 | 华南理工大学 | Application of tangeretin in preparation of medicine or health-care product for preventing and treating oral cancer |
| CN105748380A (en) * | 2016-05-05 | 2016-07-13 | 天津市聚星康华医药科技有限公司 | Full-effective repairing toothpaste containing varied functional compositions |
| CN108294984A (en) * | 2018-03-10 | 2018-07-20 | 李思敏 | A kind of clear novel toothpaste |
| CN108158913B (en) * | 2018-03-20 | 2020-10-27 | 扬州工业职业技术学院 | Sterilizing and deodorizing traditional Chinese medicine toothpaste and preparation method thereof |
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- 2018-10-29 WO PCT/CN2018/112368 patent/WO2020062389A1/en active Application Filing
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| CN101244016A (en) * | 2008-03-17 | 2008-08-20 | 柳州两面针股份有限公司 | Application of aurantiin in preparing oral cavity nursing health products |
| CN102579275A (en) * | 2012-02-22 | 2012-07-18 | 合肥学院 | Beautifying toothpaste containing aluminum-magnesium silicate and preparation method of beautifying toothpaste |
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| 吕凛等: "超临界二氧化碳萃取橘皮中黄酮类化合物的工艺研究", 《食品科学》 * |
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Application publication date: 20181123 |