CN102512344B - Blumea balsamifera extract, preparation method and application thereof in oral care and clean product - Google Patents
Blumea balsamifera extract, preparation method and application thereof in oral care and clean product Download PDFInfo
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Abstract
The invention relates to a preparation method of blumea balsamifera extract, which comprises the steps of: a) carrying out a water vapor distillation method on blumea balsamifera and respectively obtaining volatile oil, filtrate and dreg of decoction; b) drying the filtrate and obtaining water extract; c) extracting the dreg of decoction by ethanol, filtering the extracted liquid, concentrating the filtrate into thick paste with the density of 1.05 at the temperature of 60 DEG C, using ethyl acetate with the weight equal to that of the thick paste for extracting, recovering and drying the ethyl acetate, and obtaining ethyl acetate extract; and d) mixing the volatile oil, the water extract and the ethyl acetate extract, and obtaining the blumea balsamifera extract. The invention also relates to the blumea balsamifera extract prepared by the method. The invention further relates to the application of the blumea balsamifera extract in an oral care and clean product. When being added into the oral care and clean product, the blumea balsamifera extract has the functions of treating inflammation, sterilizing and clearing the throat when being used for cleaning the oral cavity in the daily life, and is especially suitable for the occasion that teeth can not be brushed or are inconvenient to brush.
Description
Technical field
The present invention relates to field of medicaments, relate in particular to Herba Blumeae Balsamiferae extract and preparation method thereof and the application in the mouth care cleaning product.
Background technology
Along with the raising day by day of living standard, people also improve gradually to the health care consciousness of self, and oral cavity health is one of them, and oral cavity health had both comprised the prior mouth care that refers to of daily oral cavity cleaning, to reach the purpose that keeps oral health.Mouth care cleaning series products in the market comprises oral nursing liquid, collutory, mouthspray, toothpaste, chewing gum etc.
Traditional oral cavity cleaning hygienic article, its basic function is cleaning teeth, fresh breath reaches the purpose that keeps oral cavity cleaning.In recent years, because the consumer healthcare realizes continuous enhancing, oral-cavity cleaning products has been proposed more requirement, also increased some auxiliary prevention oral diseases except cleaning the teeth, the oral cavity has been had the function of nursing health effect.Again because the Chinese medicinal plant active component has advantages of that the Western medicine such as natural, safe is incomparable, therefore become the emphasis of Developing on market with the functional type oral-cavity cleaning products of active ingredient of Chinese herbs.Along with the development of modernization of Chinese medicine technology, the method for Chinese medicine study of active components utilization has also been obtained good development, this assists the prevention oral disease that good technical support is provided for oral-cavity cleaning products utilizes active ingredient of Chinese herbs.
Oral inflammation, oral ulcer, aphtha are a kind of take outbreak periodically repeatedly as the oral mucosa limitation ulcer infringement of characteristics, can spontaneous recovery, can betide any position of oral mucosa, and common with lip, cheek, tongue, severe patient can involve pharyngeal mucosa.Many patients are along with the prolongation of the course of disease, and ulcer area increases, and number increases, and pain increases the weight of, and healing stage extends, and shorten interval etc., affect food and speak.Although the Therapeutic Method to stomatitis, oral ulcer, pharyngitis, laryngitis, aphtha, halitosis, periodontitis, gingivitis is a lot, but be substantially all symptomatic treatment, purpose is mainly ease the pain or reduce recurrent number, but Control in recurring fully, so the prevention primary disease is particularly important.
For specific crowd or specific occasion, do not have for various reasons conditioned disjunction not brush teeth with toothpaste, as: with after the meal, see the client before, before and after tooth treatment, or the old people of loss of tooth, the child that can not brush teeth etc., in this case, select oral nursing liquid or collutory more suitable.
Herba Blumeae Balsamiferae is the fresh or dry aerial parts of feverfew Herba Blumeae Balsamiferae Blumea balsamifera (L.) DC., be commonly called as " Na Long " (multitude's medicine name), " Balsamiferou Blumea Herb ", one of China Li nationality, Miao ethnic group's folk medicine, acrid in the mouth, hardship, warm in nature, enter liver, kidney, urinary bladder channel, have that warming middle-JIAO is invigorated blood circulation, a function of regulating menstruation, wind-damp dispelling, be used for the treatment of the diseases such as affection of exogenous wind-cold dysentery, stomachache, borborygmus, swelling, menoxenia, bones and muscles pain.Herba Blumeae Balsamiferae is mainly as the raw material that extracts Chinese mugwort powder, Blumeae preparatum Tabellae and Oleum Blumeae Balsamiferae, has long use historical, the Ming Dynasty as far back as China, the doctor among the people in Nationality in Hainan Province area applies ointment or plaster with regard to useful its blade bake and treats the experience of skin burn, weapons wound, obtain water decoction with other medical materials of the composite minority of its blade, washout treatment women expelling wind and removing dampness in puerperal, most women of the Li nationality all know this function.
Modern study shows, mainly contain volatile ingredient and flavones ingredient in Herba Blumeae Balsamiferae, mainly contain L-Borneol, β-caryophyllene, Camphora, australene, nopinene, Fructus Citri Limoniae alcohol, linalool, borneol acetate isoreactivity composition in Herba Blumeae Balsamiferae volatile oil, have respectively diaphoresis, relieving convulsion, anthelmintic, relieving asthma, heart tonifying, antitussive, eliminate the phlegm, the effect such as antibiotic, antiviral.Flavones ingredient, especially flavanone have very strong antioxidation.Department of chemistry of Zhongshan University separates from Herba Blumeae Balsamiferae and obtains blumeatin, and finds that this compound has certain cardiac vascular activity and antioxidation, anti-experimental character hepatic injury effect.By Herba Blumeae Balsamiferae extract blumeatin and chemical improvement thing thereof are carried out the research of pharmacologically active, find that this compounds has liver protective effect preferably and stronger inhibition lipid peroxidation.Flavanone in Herba Blumeae Balsamiferae has protective effect to the rat experiment liver damage, has anti-CCl
4, AAP and TAA the acute liver damage effect.Lipid peroxidation injury rat Yuan Dynasty culture hepatocyte there is protective effect.
Summary of the invention
The preparation method that the purpose of this invention is to provide a kind of Herba Blumeae Balsamiferae extract.
The present invention also aims to provide the Herba Blumeae Balsamiferae extract by the method preparation.
The present invention also aims to provide the application of this Herba Blumeae Balsamiferae extract in the mouth care cleaning product.
In order to realize purpose of the present invention, the invention provides a kind of preparation method of Herba Blumeae Balsamiferae extract, the method comprises the following steps:
A) make Herba Blumeae Balsamiferae carry out steam distillation to obtain respectively volatile oil, filtrate and medicinal residues;
B) make the described filtrate drying of step in a) to obtain water extract;
C) make the described medicinal residues ethanol extraction of step in a), with extracting liquid filtering and filtrate is concentrated into 60 ℃ of lower densities is 1.05 thick paste, extract with the ethyl acetate with the weight such as described thick paste, reclaim ethyl acetate and dry to obtain ethyl acetate extract; And
D) mix described volatile oil, described water extract and described ethyl acetate extract, thereby obtain described Herba Blumeae Balsamiferae extract.
Herba Blumeae Balsamiferae (Blumea balsamifera (L) DC) belongs to the dry herb of Herba Blumeae Balsamiferae for the Compositae Herba Blumeae Balsamiferae.Being the national common medicine use such as the Li nationality, Miao ethnic group and Zhuang, is also the plant origin of producing Blumeae preparatum Tabellae simultaneously.Main product in Guizhou, the province such as Guangxi, Yunnan and Taiwan.According to putting down in writing in " Chinese medicine voluminous dictionary ": Herba Blumeae Balsamiferae is warm in nature, and acrid in the mouth has warming middle-JIAO and invigorates blood circulation, the effect of expelling wind and removing dampness, anti-inflammatory analgesic.Cold-damp be can treat and cold-damp dysentery, the diseases such as stomachache borborygmus, traumatic injury knife injury and hypertension can be used for treating, and for diseases such as advanced menstruation, massive postpartum vaginal bleeding, puerperal edema, infertility, the erosion of vulva, curative effect is preferably arranged also, also can be used in addition burn, scald and skin injury and mosquito bite etc.Take Herba Blumeae Balsamiferae as raw material, make with extra care the Chinese mugwort oil that produces in the process of Blumeae preparatum Tabellae, have blood vessel dilating, reduce blood pressure and suppress orthosympathetic effect.
Preferably, described step a) in, operating weight is that the water soaking Herba Blumeae Balsamiferae of 8 times of Herba Blumeae Balsamiferae weight spends the night, and then is placed in together the volatile oil extractor reflux, extract.
Wherein, steam distillation is method well-known to those skilled in the art, means containing medical material and the water condistillation of volatile ingredient, and volatile ingredient is distillated in the lump with steam, divides the leach extraction method of getting volatile ingredient through condensation.This method is applicable to have volatility, can be destroyed with vapor distillation, the lixiviate of stable and indissoluble or water-fast medicinal ingredient in water.Common equipment is multifunctional extracting pot, volatile oil extraction pot, and it is widely used in activity in production.In the present invention, when going out, non-volatile oil stream stops extracting operation.
As used in this article, dehydrated alcohol and ethanol water contained in term " ethanol ".Preferably, at described step c) in, described ethanol is the ethanol water of 60-95 volume %.
More preferably, at described step c) in, described extraction comprises that cold-maceration extracts, circumfluence method is extracted and percolation extracts.
Preferably, when extracting by circumfluence method, extraction time is generally 2-4 time, and extracting solvent is the ethanol water of 60 volume %, the ethanol water of 80 volume % or the ethanol water of 95 volume %, and the extraction weight of solvent is 2-4 times of medicinal residues weight.
In the method for the invention, the inventor finds amazedly, most preferably, at described step c) in, making the described medicinal residues of step in a) carry out circumfluence method extracts 3 times, each all operating weights are the ethanol water of 95 volume % of 3 times of medicinal residues weight, and extraction time is respectively 2h, 1.5h and 1h.At the fungistatic effect under this condition significantly greater than the Herba Blumeae Balsamiferae extract for preparing under other conditions.
Preferably, at described step c) in, the ethyl acetate of the weight such as use and described thick paste extracts 3 times.
The present invention also provides the Herba Blumeae Balsamiferae extract by above-mentioned preparation.
The present invention also provides the application of described Herba Blumeae Balsamiferae extract in the mouth care cleaning product.Preferably, described mouth care cleaning product is oral nursing liquid, collutory, mouthspray, toothpaste or chewing gum.
The application of described Herba Blumeae Balsamiferae extract in oral nursing liquid is to extract with said method in the substrate that the Herba Blumeae Balsamiferae extract that obtains adds the mouth care cleaning product to, to be prepared into the mouth care cleaning product.Add mouth care cleaning series products substrate to and comprise any antiseptic or antibacterial, acid adjustment or accent alkali liquor, aromatic, excipient, dispersion diluent, toner, stabilizing agent, thickening agent, surfactant and other known conventional adjuvant that allows to be added in this series products.
The present invention has following advantage and beneficial effect with respect to prior art:
(1) Herba Blumeae Balsamiferae extract adds in oral nursing liquid and mouthspray as additive, can be at anti-inflammation and sterilization in the daily cleaning oral cavity, the effect of pharynx-clearing throat-benefiting, especially for can not or inconvenient crowd and occasion of brushing teeth with toothbrush.
(2) Herba Blumeae Balsamiferae extract adds as additive and plays the effect that slows down preferably oral inflammation, dental gingival hemorrhage symptom in toothpaste and collutory.Join the chewing gum of making in the formula of chewing gum and can fully discharge after chew in the oral cavity, and enter digestive tract with saliva, bring into play it to the protective effect of oral cavity, digestive tract and respiratory tract.
(3) Herba Blumeae Balsamiferae extract is applied in the mouth care cleaning product, and is easy to use, and treatment oral disease effect is remarkable, has no side effect, and is easy to be accepted.
(4) the Herba Blumeae Balsamiferae extract preparation method is simple, and production cost is little, adds in the mouth care cleaning product, and is little to mouth care cleaning product cost impact, still, greatly improves the use value of mouth care cleaning product aspect the mouth care cleaning.
The specific embodiment
Below the invention will be further described for the description by the specific embodiment, but this is not to be limitation of the present invention, those skilled in the art are according to basic thought of the present invention, can make various modifications or improvement, but only otherwise break away from basic thought of the present invention, all within the scope of the present invention.
In method as herein described, except as otherwise noted, otherwise described operation is all depressed at 1 standard atmosphere and is carried out.
The preparation of embodiment 1 Herba Blumeae Balsamiferae extract
Get Herba Blumeae Balsamiferae 100 grams, pulverized 40 mesh sieves after oven dry, the distilled water immersion that is 8 times of Herba Blumeae Balsamiferae weight with weight spends the night, and then is placed in volatile oil extractor and extracts, and till no longer including the volatile oil outflow, thereby obtains respectively volatile oil, filtrate and medicinal residues.Make described filtrate decompression drying to obtain the water extract of Herba Blumeae Balsamiferae.Make described medicinal residues carry out circumfluence method and extract 3 times, each all operating weights are the ethanol water of 95 volume % of 3 times of medicinal residues weight, and extraction time is respectively 2h, 1.5h and 1h.Merge extractive liquid, filters, and it is 1.05 thick paste that filtrate is concentrated into 60 ℃ of lower densities, and extract 3 times with ethyl acetate, each weight all with the weight such as described thick paste, combining extraction liquid, and the reclaim under reduced pressure ethyl acetate, drying and crushing obtains the ethyl acetate extract of Herba Blumeae Balsamiferae.Merge the water extract of Herba Blumeae Balsamiferae, ethyl acetate extract and the volatile oil of Herba Blumeae Balsamiferae, obtain Herba Blumeae Balsamiferae extract 18 grams.
The preparation of embodiment 2 Herba Blumeae Balsamiferae extracts
Prepare Herba Blumeae Balsamiferae extract according to the mode identical with embodiment 1, difference is to make medicinal residues to carry out reflux, extract, 2 times, and each all operating weights are the ethanol water of 60 volume % of 4 times of medicinal residues weight, and extraction time is respectively 2h and 1.5h.
The preparation of embodiment 3 Herba Blumeae Balsamiferae extracts
Prepare Herba Blumeae Balsamiferae extract according to the mode identical with embodiment 1, difference is to make medicinal residues to carry out reflux, extract, 4 times, and each all operating weights are the ethanol water of 80 volume % of 2 times of medicinal residues weight, and extraction time is respectively 2h, 1.5h, 1h and 0.5h.
The preparation of embodiment 4 Herba Blumeae Balsamiferae extracts
Prepare Herba Blumeae Balsamiferae extract according to the mode identical with embodiment 1, difference is to make medicinal residues to carry out reflux, extract, 2 times, and each all operating weights are the ethanol water of 80 volume % of 2 times of medicinal residues weight, and extraction time is respectively 2h and 1.5h.
The preparation of embodiment 5 Herba Blumeae Balsamiferae extracts
Prepare Herba Blumeae Balsamiferae extract according to the mode identical with embodiment 1, difference is to make medicinal residues to carry out reflux, extract, 4 times, and each all operating weights are the ethanol water of 60 volume % of 4 times of medicinal residues weight, and extraction time is respectively 2h, 1.5h, 1h and 0.5h.
Test example 1
Because antibacterial main in the oral cavity is staphylococcus aureus and Candida albicans, therefore investigate its application in the mouth care cleaning product by the bacteriostatic test of Herba Blumeae Balsamiferae extract of the present invention.
Bacteriostatic test
Adopt filter paper method classical in this area to carry out bacteriostatic test, wherein:
1. material
1.1 for the examination strain
Staphylococcus aureus (Staphylococcus aureus) ATCC 25923, Candida albicans (Candida albicans) ACTT 12228 is all available from Products in China calibrating institute.
1.2 culture fluid
Nutrient agar and nutrient broth are all available from BeiJing ZhongKe's space in morning experimental facilities company limited.
1.3 test method
Take respectively Herba Blumeae Balsamiferae extract 1 gram in embodiment 1 to 5, after water dissolution filtration with 8 grams, deionized water dilution with 15 grams, add successively the sodium chloride of 1.5 grams, the dehydrated alcohol of 1.5 grams, the glycerol of 3 grams, the polysorbas20 of 0.3 gram, the aspartame of 0.05 gram, the sodium carboxymethyl cellulose mixing and stirring of 0.3 gram, the last deionized water that adds again 80 grams, thus collutory 1 to 5 made.
Staphylococcus aureus and Candida albicans are inoculated on agar plate nutritional solution plane, evenly gather during inoculation.The aseptic circular filter paper sheet of tweezer uses respectively collutory 1 to 5.Filter paper is moistening, make filter paper vertical when standing drop on it just begun to drip.Filter paper is attached on the culture fluid of inoculated bacteria.Agar plate is placed in the incubator of 37 ℃ incubation 24 hours.Measure the diameter of antibacterial ring.Measuring 3 times averages.
1.4 the results are shown in following table
The diameter of antibacterial ring is larger, shows that bacteriostasis is stronger.From upper table as seen, the effect of the collutory 1 of the Herba Blumeae Balsamiferae extract of embodiment 1 is significantly higher than the effect of collutory of the Herba Blumeae Balsamiferae extract of other embodiment unexpectedly.
The preparation of embodiment 6 Herba Blumeae Balsamiferae extracts
Prepare Herba Blumeae Balsamiferae extract according to the mode identical with embodiment 1, it is 1.10 thick paste that difference is filtrate is concentrated into 60 ℃ of lower densities, thereby obtains Herba Blumeae Balsamiferae extract 12 grams.
The preparation of embodiment 7 Herba Blumeae Balsamiferae extracts
Prepare Herba Blumeae Balsamiferae extract according to the mode identical with embodiment 1, it is 1.20 thick paste that difference is filtrate is concentrated into 60 ℃ of lower densities, thereby obtains Herba Blumeae Balsamiferae extract 10 grams.
Embodiment 8 Herba Blumeae Balsamiferae extracts add in oral nursing liquid substrate
Take Herba Blumeae Balsamiferae extract 1 gram in embodiment 1, water dissolution with 8 grams, deionized water dilution with 15 grams, add the vitamin C of 0.1 gram, the hibitane of 0.01 gram, the PEG400 of 1 gram, the Aspartame of 0.02 gram, the glycerol of 1.5 grams, the Mentholum of 0.01 gram, the dehydrated alcohol of 0.1 gram, mixing and stirring, the water that adds again 75 grams, adding at last the sodium dihydrogen phosphate adjusting pH value of 0.002 gram is 8, sterilization filling.
Embodiment 9 Herba Blumeae Balsamiferae extracts add in oral spray substrate
Take the xylitol of Herba Blumeae Balsamiferae extract 2 grams in embodiment 1,0.1 gram water solublity Herba Menthae brain, 0.1 gram Aspartame, 0.2 gram dehydrated alcohol, 2 grams, be dissolved in the deionized water of 100 grams, in sterile filling and sprayer bottle.
Embodiment 10 Herba Blumeae Balsamiferae extracts add in toothpaste matrix
Take Herba Blumeae Balsamiferae extract 3 grams in embodiment 1, with the deionized water dissolving of 15 grams, filter.Deionized water with 8 grams dilutes filtrate again, add successively the insoluble Polymeric sodium metaphosphate. of 40 grams, the dicalcium phosphate dihydrate of 5 grams, the aluminium hydroxide of 3 grams, the glycerol of 20 grams, the titanium dioxide of 1 gram, the sodium benzoate of 0.6 gram, the N-sodium lauroyl sarcosine of 3 grams, the aspartame of 005 gram, the Oleum menthae of 0.05 gram, add again at last 1.3 gram deionized water and stirring mixings and get final product.
Embodiment 11 Herba Blumeae Balsamiferae extracts add in chewing gum substrate
Take Herba Blumeae Balsamiferae extract 3 grams in embodiment 1, the hydroxypropyl amylcose acetate of 20 grams, the corn syrup (430 Baume degrees) of 75 grams, the water of 1.6 grams and the glycerol of 0.2 gram and be heated to 80 ℃ in stainless-steel pan, mix homogeneously, cool to the Herba Menthae Rotundifoliae mixing that adds 0.2 gram after 60 ℃, and be divided into while hot the spherolite of 2.5 grammes per square metres, sprinkle xylosic alcohol powder for each beadlet; After placing 3 hours under the relative humidity of room temperature and 45%, packing.
Claims (6)
1. the preparation method of a Herba Blumeae Balsamiferae extract, the method comprises the following steps:
A) make Herba Blumeae Balsamiferae carry out steam distillation to obtain respectively volatile oil, filtrate and medicinal residues;
B) make the described filtrate drying of step in a) to obtain water extract;
C) make the described medicinal residues ethanol extraction of step in a), with extracting liquid filtering and filtrate is concentrated into 60 ℃ of lower densities is 1.05 thick paste, extract with the ethyl acetate with weight such as described thick pastes, reclaim ethyl acetate and dry to obtain ethyl acetate extract, wherein making the described medicinal residues of step in a) carry out circumfluence method extracts 3 times, each all operating weights are the ethanol water of 95 volume % of 3 times of medicinal residues weight, and extraction time is respectively 2h, 1.5h and 1h; And
D) mix described volatile oil, described water extract and described ethyl acetate extract, thereby obtain described Herba Blumeae Balsamiferae extract.
2. method according to claim 1, is characterized in that, described step a) in, operating weight is that the water soaking Herba Blumeae Balsamiferae of 8 times of Herba Blumeae Balsamiferae weight spends the night, and then is placed in together the volatile oil extractor reflux, extract.
3. method according to claim 1 and 2, is characterized in that, at described step c) in, the ethyl acetate of the weight such as use and described thick paste extracts 3 times.
4. one kind is passed through the Herba Blumeae Balsamiferae extract that in claims 1 to 3, the described method of any one prepares.
5. the application of Herba Blumeae Balsamiferae extract claimed in claim 4 in preparation mouth care cleaning product.
6. application according to claim 5, is characterized in that, described mouth care cleaning product is oral nursing liquid, mouthspray, toothpaste or chewing gum.
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| CN105193665A (en) * | 2015-10-26 | 2015-12-30 | 中国热带农业科学院热带作物品种资源研究所 | Blumea balsamifera oral care solution, and preparation method and application thereof |
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| CN112870115B (en) * | 2021-02-25 | 2023-04-14 | 中国热带农业科学院热带作物品种资源研究所 | Special-effect south medicine compound toothpaste for middle-aged and elderly people and preparation method thereof |
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| CN102512344A (en) | 2012-06-27 |
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