CN106377481A - Extraction method of cyperus rotundus extract and toothpaste and mouth wash containing cyperus rotundus extract - Google Patents
Extraction method of cyperus rotundus extract and toothpaste and mouth wash containing cyperus rotundus extract Download PDFInfo
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- CN106377481A CN106377481A CN201611012343.5A CN201611012343A CN106377481A CN 106377481 A CN106377481 A CN 106377481A CN 201611012343 A CN201611012343 A CN 201611012343A CN 106377481 A CN106377481 A CN 106377481A
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- rhizoma cyperi
- seed extract
- cyperus rotundus
- concentrate
- cyperi seed
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/89—Cyperaceae (Sedge family)
- A61K36/8905—Cyperus (flatsedge)
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/005—Antimicrobial preparations
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation 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
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation 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
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
Abstract
The invention relates to the technical field of plant extraction and application, in particular to an extraction method of a cyperus rotundus extract and toothpaste and mouth wash containing the cyperus rotundus extract. The extraction method of the cyperus rotundus extract comprises the following steps of (1) ultrasonic-microwave cooperated extraction; (2) concentration; (3) column chromatography separation; (4) concentration, and vacuum freeze drying, so as to obtain light yellow or light brown powder, namely the cyperus rotundus extract. The preparation method has the advantages that the pure natural traditional Chinese medicine of cyperus rotundus is extracted and purified, so that the obtained cyperus rotundus extract has an obvious inhibiting function on streptococcus mutans and porphyromonas gingivalis; the cyperus rotundus extract can be used as an active ingredient and be added into oral care articles for preventing and controlling tooth pain and gingival bleeding, such as the toothpaste, the mouth wash, tooth powder, throat lozenge and gum, the obvious functions of pain relieving and bleeding stopping are realized, the prevention function is realized, and the comprehensive health of oral cavity is maintained.
Description
Technical field
The present invention relates to plant extract and applied technical field and in particular to a kind of extracting method of rhizoma cyperi seed extract and
Toothpaste containing this rhizoma cyperi seed extract and mouthwash.
Background technology
The oral care product that people commonly use is mainly toothpaste, gargle, tooth powder, throat lozenge, chewing gum etc., its basic function
Exactly clean tooth, protect gum, safeguard the hygiene and health in oral cavity.With the continuous improvement of people's living standard, consumer couple
The security of product is increasingly paid close attention to, thus increasingly advocating natural and safe product.Interpolation can effectively prevent and treat various oral cavities
The oral care product of disease Chinese herbal medicine, little with its toxic and side effect, green, environmental protection, safe the features such as and be subject to people again
Favor, the consumption demand of this kind of product on market increases continuous.In addition, with the development of modernization of Chinese medicine technology, to Chinese medicine
The method of active component developmental research has also obtained fine development, and this is assisted pre- for oral care product using active ingredient of Chinese herbs
Anti- mouth disease provides good technical support.
Toothache is the mouth disease being caused by many reasons, shows according to relevant information, and China has more than more than 50% consumption
There is different degrees of toothache in different times in person.Bleeding gums are also one of department of stomatology common sympton, refer to that gum is spontaneous
Or because what minimal irritation caused bleeds on a small quantity.The lighter shows as carrying only in the saliva when sucking, brushing teeth, chew harder food
There is the trace of blood, severe one is that bleeding is more or even hematostaxis when gum is subject to minimal irritation.In general, the chronic inflammation of gum
Disease is the common cause of bleeding gums, therefore bleeding gums are more common in periodontitis and carious tooth inflammation patient.Porphyromonas gingivalis
(Porphyromonas gingivalis, P.gingivalis], it is a kind of Gram-negative anaerobism coccobacillus of non-glycolysis sugar.
Porphyromonas gingivalis produce multiple with pathogenic relevant virulence factor, be current research extensive and sufficient evidence cause tooth
One of the main pathogenic fungi of Zhou Yan.Research in recent years finds, also serious with the many systematicness of porphyromonas gingivalis infection
Disease, the such as correlation such as atherosclerotic and diabetes.Streptococcus mutans (Strept DEG C DEG C of cus mutans, S.
Mutans), a kind of strict anaerobes, is one of important cariogenic bacteria in oral cavity, has stronger Adhering capacity to smooth surface,
Can be colonized and be formed bacterial plaque in sticking of facing, then cariogenic.
Rhizoma cyperi（Cyperus rotundus tubers）, another name cyperi rhizoma, the rhizome of nutgrass flatsedge, incense additionaling rice, sparrow head are fragrant, Thunder God is first-class, are
Cyperaceae herbaceos perennial nutgrass flatsedge（Cyperus rotundus L.）Dry rhizome.The rhizoma cyperi bought in shop of Chinese medicines
Shape such as spindle, or slightly bend, long 2-3 centimetre, about 1 centimetre of diameter, surface is in sepia or pitchy, and has irregular
Vertical wrinkle, has special fragrance.Matter is hard, through boiling person's section yellowish-brown, cutin sample；Sun-dried person's section shows mealiness, endodermis ring
Substantially, center pillar has point-like vascular bundle to be dispersed in line.Gas is fragrant, mildly bitter flavor.Rhizoma cyperi taste is pungent, slight bitter, micro-sweet, mild-natured, Return liver, tri-jiao channel,
It is soothing liver-qi stagnation, menstruction regulating and pain relieving, the good merchantable brand of promoting the circulation of qi solution silt.The rhizome of nutgrass flatsedge is conventional Chinese medicine, but the extraction with regard to its extract
Method is different, the drug effect obtaining also very different, and the other application field for the rhizome of nutgrass flatsedge is not yet open too many at present.
Content of the invention
In order to overcome shortcoming and defect present in prior art, it is an object of the invention to provide a kind of rhizome of nutgrass flatsedge is extracted
The extracting method of thing, extraction efficiency is high, and active constituent content is high, and process is simple is easy to operate.
It is an object of the invention to provide a kind of application of rhizoma cyperi seed extract, it can be added to toothpaste, mouthwash, tooth
In powder, chewing gum, throat lozenge, Streptococcus mutans ATCC 25175 and porphyromonas gingivalis ATCC 33277 is had significantly
Inhibitory action.
It is an object of the invention to provide a kind of toothpaste of rhizoma cyperi seed extract, there is anti-inflammation and sterilization, prevent the work of carious tooth
With.
It is an object of the invention to provide a kind of mouthwash of rhizoma cyperi seed extract, there is anti-inflammation and sterilization, prevent carious tooth
Effect.
The purpose of the present invention is achieved through the following technical solutions：
A kind of extracting method of rhizoma cyperi seed extract, comprises the following steps：
1）Ultrasonic-microwave is worked in coordination with and is extracted：The granularity being dried is 150-300 μm of rhizome of nutgrass flatsedge powder and 80wt%-95wt%
Ethanol solution puts in the lump in Ultrasonic-microwave synergistic extraction equipment cavity and is extracted, and extracts 2-4 time；Cool down after the completion of extraction,
Screen filtration extract using 150-200 mesh obtains filtrate, merging filtrate；Described ethanol solution quality is described rhizome of nutgrass flatsedge powder
6-8 times of last quality；
2）Concentrate：Described filtrate is concentrated, removes the ethanol in extract, be then centrifuged for obtaining concentrate；
3）Pillar layer separation：Concentrate after described centrifugation is passed through chromatographic column, first with the 10wt%-20wt% of 2-6 times of column volume
Ethanol or water elution impurity, then the 30wt%-50wt% ethanol elution with 2-6 times of column volume collect eluent；
4）Concentrate：By step 3）In the eluent that obtains concentrated, remove the ethanol in concentrate, the concentrate obtaining is carried out
Centrifugation, then be dried with vacuum freeze drier, the light yellow or light brown powder obtaining is rhizoma cyperi seed extract.
Wherein, described step 1）Described in ultrasonic-microwave work in coordination with extract when condition be：Ultrasonic power is 40-350W,
Microwave power is 10-500W, and Extracting temperature is 50-70 DEG C, and extraction time is 30min-60min.
Wherein, described step 2）Step 4) in centrifugation when centrifugation rate be 4000-10000rpm, the time be 10-
30min.
Wherein, described step 2）With 4）The condition of middle concentration is：Pressure is -0.08MPa～-0.09Mpa, and temperature is 45
℃-60℃ .
Wherein, described step 4) in vacuum freeze drying when, temperature：- 80～-85 DEG C, pressure 1-8pa, time 24-40h.
Wherein, described step 3）Filler in middle chromatographic column is polyamide or macroporous absorbent resin, and amount of filler is
1-5 times of described supernatant quality, the blade diameter length ratio 1 of described filler：4-1：8, adsorption flow rate is 0.5-6.0BV/h, elution flow rate
For 0.5～6.0BV/h.The type of described macroporous absorbent resin is AB-8, one of D-101, HDP-100C, SP-825.
Wherein, described step 2）Middle employing reduced pressure concentration, concentrate and step 1 raw material when described filtrate is concentrated into 25 DEG C
Rhizome of nutgrass flatsedge powder quality is than for 2:1；Described step 4）Middle employing reduced pressure concentration, described eluent is carried out being concentrated into dense when 25 DEG C
Contracting liquid and step 1 raw material rhizome of nutgrass flatsedge powder quality are than for 10:1.
A kind of application of rhizoma cyperi seed extract, be added to toothpaste, mouthwash, tooth powder, chewing gum, in throat lozenge, its interpolation
Measure as 0.1-5%.
A kind of toothpaste containing rhizoma cyperi seed extract, comprises the following raw materials by weight percent：
Rhizoma cyperi seed extract 5.0%
Sorbierite 18.0%
Propane diols 2.0%
Glycerine 2.0%
Sodium carboxymethylcellulose 1.2%
Guar gum 0.2%
Saccharin sodium 0.2%
Essence 1.0%
Lauryl sodium sulfate 2.0%
Calcite in powder 38.0%
Silica 4.0%
Nipalgin mixed ester sodium 0.15%
Deionized water surplus.
A kind of mouthwash containing rhizoma cyperi seed extract, comprises the following raw materials by weight percent：
Rhizoma cyperi seed extract 1%
Sorbierite 22%
Food grade ethanol 10%
Rilanit special -40 0.8%
Saccharin sodium 0.01%
Essence 0.6%
Nipalgin mixed ester sodium 0.15%
Deionized water surplus %.
The concentration of herein described ethanol water is the aqueous solution of ethanol volumn concentration percentage.
Heretofore described rhizoma cyperi seed extract all taking the pure extract powder that active component is 100% as a example, but not
It is limited as the other forms such as pure extract powder or extract or medicinal extract.As extract, it is applied to mouth when otherwise
When the nursing product of chamber, the addition in formula should be converted to disclosed in this invention pure form of extract amount.
Beneficial effects of the present invention：A kind of present invention environmental friendliness, efficiently, no with the Chinese herbal medicine rhizome of nutgrass flatsedge as development of raw materials
The potential novel mouth bacterial inhibitor of poison, has far-reaching significance to ecological long term growth, the health of Human Oral Cavity and all.With
Traditional oral care product additive is compared, and the present invention has the characteristics that following and advantage：1st, the rhizome of nutgrass flatsedge of the present invention is extracted
Thing, has obvious inhibitory action to Streptococcus mutans ATCC 25175 and porphyromonas gingivalis ATCC 33277.2nd, this
Bright rhizoma cyperi seed extract is not overlapping with health-care components α in the rhizome of nutgrass flatsedge-cyperolone place polar fraction, does not affect rhizome of nutgrass flatsedge medicine
The use of effect composition, can become and exploit natural resources well.
The present invention carries out extraction and purification process using the pure natural Chinese medicine rhizome of nutgrass flatsedge, and the rhizoma cyperi seed extract obtaining is to variation
Streptococcus ATCC 25175 and porphyromonas gingivalis ATCC 33277 has obvious inhibitory action, thus can become as activity
Divide in the oral care implement being added to special preventing and treating toothache and bleeding gums, such as toothpaste, gargle, tooth powder, throat lozenge, mouth
Fragrant sugar etc., has obvious analgesia and anastalsis, prevents and safeguard oral cavity total health.
Specific embodiment
For the ease of the understanding of those skilled in the art, with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying refers to not limitation of the invention.
Embodiment 1
Take 100g rhizome of nutgrass flatsedge raw material, be dried the powder for 200 μm of granularity, add the ethanol solution of 600g80 wt % in the lump
Put in Ultrasonic-microwave synergistic extraction equipment cavity and extracted, ultrasonic power is 100W, microwave power is 50W, extracts temperature
Spend for 60 DEG C, extraction time is 60min, extracts 3 times；Cool down after the completion of extraction, the screen filtration extract using 150 mesh obtains
Filtrate, merging filtrate, in pressure -0.09Mpa, temperature is to be concentrated into 50g, then under the rotating speed of 5000rpm/min when 60 DEG C
Centrifugation 15min；By the concentrate after centrifugation, by the polyamide of 80 mesh, first with 10wt% ethanol or the water of 3 times of column volumes
Wash-out impurity, then 30 wt % ethanol elutions with 3 times of column volumes collect eluent；Eluent is concentrated and is centrifuged,
Pressure -0.09Mpa, temperature is to be concentrated into 10g when 55 DEG C, is then centrifuged 20min under the rotating speed of 6000rpm/min, in temperature
- 80 DEG C of degree, pressure 2pa, freeze-drying 30h.The light yellow or light brown powder obtaining is rhizoma cyperi seed extract 6g.
Embodiment 2
Take 200g rhizome of nutgrass flatsedge raw material, be dried the powder for 300 μm of granularity, add the ethanol solution of 1600g90 wt % in the lump
Put in Ultrasonic-microwave synergistic extraction equipment cavity and extracted, ultrasonic power is 100W, microwave power is 100W, extracts
Temperature is 55 DEG C, and extraction time is 50min, extracts 2 times；Cool down after the completion of extraction, the screen filtration extract using 200 mesh obtains
To filtrate, merging filtrate, in pressure -0.09Mpa, temperature is to be concentrated into 100g when 60 DEG C, then turning in 6000rpm/min
Speed is lower to be centrifuged 20min；By the concentrate after centrifugation, by macroreticular resin AB-8, first with 10wt% ethanol or the water of 3 times of column volumes
Wash-out impurity, then 30 wt % ethanol elutions with 3 times of column volumes collect eluent；Eluent is concentrated and is centrifuged,
Pressure -0.08Mpa, temperature is to be concentrated into 20g when 50 DEG C, is then centrifuged 15min under the rotating speed of 5000rpm/min, in temperature
- 80 DEG C of degree, pressure 2pa, freeze-drying 35h.The light yellow or light brown powder obtaining is rhizoma cyperi seed extract 12g.
Embodiment 3
Take 300g rhizome of nutgrass flatsedge raw material, be dried the powder for 150 μm of granularity, add the ethanol solution of 2100g85 wt % in the lump
Put in Ultrasonic-microwave synergistic extraction equipment cavity and extracted, ultrasonic power is 150W, microwave power is 100W, extracts
Temperature is 60 DEG C, and extraction time is 60min, extracts 3 times；Cool down after the completion of extraction, the screen filtration extract using 150 mesh obtains
To filtrate, merging filtrate, in pressure -0.09Mpa, temperature is to be concentrated into 50g, then in the rotating speed of 5000rpm/min when 60 DEG C
Lower centrifugation 15min；By the concentrate after centrifugation, by macroreticular resin D-101, first with 10wt% ethanol or the washing of 3 times of column volumes
Removing impurities matter, then 30 wt % ethanol elutions with 3 times of column volumes collect eluent；Eluent is concentrated and is centrifuged, in pressure
Power -0.09Mpa, temperature be 55 DEG C when be concentrated into 10g, then under the rotating speed of 5000rpm/min be centrifuged 20min, temperature -
80 DEG C, pressure 2pa, freeze-drying 35h.The light yellow or light brown powder obtaining is rhizoma cyperi seed extract 18g.
Embodiment 4
Take 400g rhizome of nutgrass flatsedge raw material, be dried the powder for 200 μm of granularity, add the ethanol solution of 2400g95 wt % in the lump
Put in Ultrasonic-microwave synergistic extraction equipment cavity and extracted, ultrasonic power is 100W, microwave power is 150W, extracts
Temperature is 60 DEG C, and extraction time is 60min, extracts 4 times；Cool down after the completion of extraction, the screen filtration extract using 150 mesh obtains
To filtrate, merging filtrate, in pressure -0.09Mpa, temperature is to be concentrated into 200g when 60 DEG C, then turning in 5000rpm/min
Speed is lower to be centrifuged 15min；By the concentrate after centrifugation, by macroreticular resin HPD-100C, first with the 10wt% ethanol of 3 times of column volumes
Or water elution impurity, then 30 wt % ethanol elutions with 5 times of column volumes collect eluent；Eluent is concentrated and from
The heart, in pressure -0.09Mpa, temperature is to be concentrated into 40g when 60 DEG C, is then centrifuged 30min under the rotating speed of 7000rpm/min,
In -80 DEG C of temperature, pressure 2pa, freeze-drying 40h.The light yellow or light brown powder obtaining is rhizoma cyperi seed extract
24g.
Antibiotic property detects
Anaerobism challenge experiment in the present invention, uses agar plate dilution method, comprises the following steps that：Activated strains；Pass
Culture；Prepare bacteria suspension；Prepare sample；Preparation band medicine flat board；Measure bacteriostatic activity.
Antibacterial effect test result is as shown in the table
| Title | Concentration（mg/ml） | Streptococcus mutans 25175MIC（mg/ml） | Porphyromonas gingivalis 33277MIC（mg/ml） |
| Blank | 0 | ++ | ++ |
| 0.3 | ++ | ++ | |
| 0.6 | + | + | |
| Embodiment 1 | 0.9 | — | — |
| 1.2 | — | — | |
| 1.5 | — | — | |
| 0.5 | ++ | ++ | |
| 0.7 | + | + | |
| Embodiment 2 | 0.9 | — | — |
| 1.1 | — | — | |
| 1.3 | — | — | |
| 0.7 | ++ | ++ | |
| 0.8 | + | + | |
| Embodiment 3 | 0.9 | — | — |
| 1 | — | — | |
| 1.1 | — | — | |
| 0.6 | ++ | ++ | |
| 0.7 | ++ | ++ | |
| Embodiment 4 | 0.8 | + | + |
| 0.9 | — | — | |
| 1 | — | — |
The results show, rhizoma cyperi seed extract is to Streptococcus mutans ATCC 25175 and porphyromonas gingivalis ATCC 33277
Low concentration is no obvious inhibiting effect, more than 1mg/ml, has obvious inhibitory action, and MIC is 0.9-1mg/
ml.
Above-mentioned rhizoma cyperi seed extract is preparing Streptococcus mutans ATCC 25175 and porphyromonas gingivalis ATCC 33277
Application in inhibitor, the various raw rhizome ofs nutgrass flatsedge, the rhizome of nutgrass flatsedge processed are preparing Streptococcus mutans ATCC 25175 and/or porphyromonas list
Application in born of the same parents bacterium ATCC 33277 inhibitor falls within protection scope of the present invention.Become with above-mentioned rhizome of nutgrass flatsedge extract for activity
The pathogenetic bacteria inhibitor dividing falls within protection scope of the present invention；Described pathogenetic bacteria is Streptococcus mutans ATCC 25175
And/or two kinds in porphyromonas gingivalis ATCC 33277 or a kind of.
Embodiment 5
A kind of toothpaste containing rhizoma cyperi seed extract, comprises the following raw materials by weight percent：
Rhizoma cyperi seed extract 5.0%
Sorbierite 18.0%
Propane diols 2.0%
Glycerine 2.0%
Sodium carboxymethylcellulose 1.2%
Guar gum 0.2%
Saccharin sodium 0.2%
Essence 1.0%
Lauryl sodium sulfate 2.0%
Calcite in powder 38.0%
Silica 4.0%
Nipalgin mixed ester sodium 0.15%
Deionized water surplus.
Lotion of toothpaste is made using the one-step method cream production technology of conventional medicine toothpaste：Temporary cylinder puts into and measures
Pure water, sorbierite, the liquid material such as rhizoma cyperi seed extract；The calcite in powder measuring, saccharin sodium, carboxylic is put in pre-dispersed kettle
Base sodium cellulosate, lauryl sodium sulfate, nipalgin mix the powders such as ester sodium, carry out pre-dispersed, mixing；Open cream kettle vacuum pumping processed
Enter above-mentioned liquid material；Then open scraper, enter above-mentioned powder, drive agitator and colloid mill, put into essence after 30 minutes, after 10 minutes
Close colloid mill, agitator, scraper, vacuum breaker successively, stop vavuum pump, make after sampling detection is qualified, sterilization filling.
Embodiment 6
A kind of mouthwash containing rhizoma cyperi seed extract, comprises the following raw materials by weight percent：
Rhizoma cyperi seed extract 1%
Sorbierite 22%
Food grade ethanol 10%
Rilanit special -40 0.8%
Saccharin sodium 0.01%
Essence 0.6%
Nipalgin mixed ester sodium 0.15%
Deionized water surplus %.
First rhizoma cyperi seed extract, nipalgin mixed ester sodium are added stirring and dissolving in edible ethanol to be placed in temporary pot, will
Sorbierite, deionization, rilanit special -40 add stirring 10 minutes in agitated kettle, the ethanol solution in temporary pot is added and stirs
Mix in pot and stir 10 minutes, be eventually adding essence and stir 5 minutes, stop stirring, make after sampling detection is qualified, sterilization filling.
Volunteer tests
The toothpaste of the rhizoma cyperi seed extract extracting containing the present invention prepared by the present invention is treating alleviated gingivitis symptom with gargling
Clinical effectiveness basic condition is as follows：Choose volunteer 100 people, men and women half and half, one full year of life at age 18-60, average age 30 one full year of life, tool
Have that gingivitis, carious tooth are scorching, have a toothache, the symptom such as bleeding gums.Using the toothpaste containing rhizoma cyperi seed extract, sooner or later use, use
Time is 6 months, and 68 people's symptoms substantially mitigate, and several individuals thoroughly solve oral problem, efficient reaches 70%.
The oral care implement of the rhizoma cyperi seed extract preparation of the present invention is applicable to various people, to gingivitis, carious tooth
Scorching, have a toothache, the symptom such as bleeding gums has good therapeutic effect, using rear no allergic reaction and have no toxic side effect, Er Qiejian
Effect is fast, and effect is good, simple and convenient, and men and women, old and young all can use.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can be realized with alternate manner,
Without departing from obvious replacement any on the premise of present inventive concept all within protection scope of the present invention.
Claims (10)
1. a kind of extracting method of rhizoma cyperi seed extract it is characterised in that：Comprise the following steps：
1）Ultrasonic-microwave is worked in coordination with and is extracted：The granularity being dried is 150-300 μm of rhizome of nutgrass flatsedge powder and 80wt%-95wt%
Ethanol solution puts in the lump in Ultrasonic-microwave synergistic extraction equipment cavity and is extracted, and extracts 2-4 time；Cool down after the completion of extraction,
Screen filtration extract using 150-200 mesh obtains filtrate, merging filtrate；Described ethanol solution quality is described rhizome of nutgrass flatsedge powder
6-8 times of last quality；
2）Concentrate：Described filtrate is concentrated, removes the ethanol in extract, be then centrifuged for obtaining concentrate；
3）Pillar layer separation：Concentrate after described centrifugation is passed through chromatographic column, first with the 10wt%-20wt% of 2-6 times of column volume
Ethanol or water elution impurity, then the 30wt%-50wt% ethanol elution with 2-6 times of column volume collect eluent；
4）Concentrate：By step 3）In the eluent that obtains concentrated, remove the ethanol in concentrate, the concentrate obtaining is carried out
Centrifugation, then be dried with vacuum freeze drier, the light yellow or light brown powder obtaining is rhizoma cyperi seed extract.
2. a kind of rhizoma cyperi seed extract according to claim 1 extracting method it is characterised in that：Described step 1）Middle institute
When stating ultrasonic-microwave collaborative extraction, condition is：Ultrasonic power is 40-350W, and microwave power is 10-500W, Extracting temperature
For 50-70 DEG C, extraction time is 30min-60min.
3. a kind of rhizoma cyperi seed extract according to claim 1 extracting method it is characterised in that：Described step 2）Step
4) in, during centrifugation, centrifugation rate is 4000-10000rpm, and the time is 10-30min.
4. a kind of rhizoma cyperi seed extract according to claim 1 extracting method it is characterised in that：Described step 2）With 4）
The condition of middle concentration is：Pressure is -0.08MPa～-0.09Mpa, and temperature is 45 DEG C -60 DEG C.
5. a kind of rhizoma cyperi seed extract according to claim 1 extracting method it is characterised in that：Described step 4) in true
During vacuum freecing-dry, temperature：- 80～-85 DEG C, pressure 1-8pa, time 24-40h.
6. a kind of rhizoma cyperi seed extract according to claim 1 extracting method it is characterised in that：Described step 3）Middle color
Filler in spectrum post is polyamide or macroporous absorbent resin, and amount of filler is 1-5 times of described supernatant quality, described fills out
The blade diameter length ratio 1 of material：4-1：8, adsorption flow rate is 0.5-6.0BV/h, and elution flow rate is 0.5～6.0BV/h.
7. a kind of rhizoma cyperi seed extract according to claim 1 extracting method it is characterised in that：Described step 2）In adopt
With reduced pressure concentration, when described filtrate is concentrated into 25 DEG C, concentrate and raw material rhizome of nutgrass flatsedge powder quality are than for 2:1；Described step 4）
Middle employing reduced pressure concentration, when described eluent is carried out being concentrated into 25 DEG C, concentrate and raw material rhizome of nutgrass flatsedge powder quality are than for 10:
1.
8. the rhizoma cyperi seed extract described in a kind of any one of claim 1-7 application it is characterised in that：It is added to toothpaste, gargle
In saliva, tooth powder, chewing gum, throat lozenge, its addition is 0.1-5%.
9. the rhizoma cyperi seed extract described in a kind of any one containing claim 1-8 toothpaste it is characterised in that：By following weight
The raw material composition of percentage：
Rhizoma cyperi seed extract 5.0%
Sorbierite 18.0%
Propane diols 2.0%
Glycerine 2.0%
Sodium carboxymethylcellulose 1.2%
Guar gum 0.2%
Saccharin sodium 0.2%
Essence 1.0%
Lauryl sodium sulfate 2.0%
Calcite in powder 38.0%
Silica 4.0%
Nipalgin mixed ester sodium 0.15%
Deionized water surplus.
10. the rhizoma cyperi seed extract described in a kind of any one containing claim 1-8 mouthwash it is characterised in that：By following
The raw material composition of percentage by weight：
Rhizoma cyperi seed extract 1%
Sorbierite 22%
Food grade ethanol 10%
Rilanit special -40 0.8%
Saccharin sodium 0.01%
Essence 0.6%
Nipalgin mixed ester sodium 0.15%
Deionized water surplus %.
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| CN201611012343.5A CN106377481B (en) | 2016-11-17 | 2016-11-17 | A method for extracting rhizoma Cyperi extract, and toothpaste and collutory containing the same |
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| CN106377481B (en) | 2020-11-20 |
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