CN101558808A - Soft capsule of camellia chrysantha tea and preparation method thereof - Google Patents
Soft capsule of camellia chrysantha tea and preparation method thereof Download PDFInfo
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- CN101558808A CN101558808A CNA2009101140408A CN200910114040A CN101558808A CN 101558808 A CN101558808 A CN 101558808A CN A2009101140408 A CNA2009101140408 A CN A2009101140408A CN 200910114040 A CN200910114040 A CN 200910114040A CN 101558808 A CN101558808 A CN 101558808A
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Abstract
The invention relates to a soft capsule which is prepared by using camellia chrysantha tea leaves to extract effective substances. The soft capsule comprises the main materials of camellia chrysantha tea extract, vegetable oil and beeswax; a preparation method comprises the following steps of: extracting saponin from fresh leaves of the camellia chrysantha tea, carrying out separation and purification, spraying, drying and obtaining saponin fine powder of the camellia chrysantha tea. The saponin fine powder of the camellia chrysantha tea, vegetable oil and beewax are prepared into mixed suspended matter according to 1:1:0.02; rubber sheet is prepared by gelatin, glycerin and water with the proportion of 1:0.35:0.9; then the mixed suspended matter is filled and pressed into the soft capsule which is shaped below the temperature of 25 DEG C; the alcohol is used for cleaning and removing the outer oil layer of the soft capsule; and the obtained object is dried under the temperature of 25 DEG C, and taken out, thus obtaining the soft capsule. The soft capsule has obvious functions of resisting oxidation and aging, beautifying skin, improving immunity of organisms and the like, is suitable for being eaten by sub-health crowds and has obvious health effect.
Description
Technical field
The invention belongs to the health product of making from the plant extract material, particularly soft capsule and the production method of making from the material of plant golden camellia tea extraction thereof.
Background technology
Camellia nitidissima [Camellia chrysantha (Hu) Tuyama] is Theaceae, Camellia, Camellia nitidissima group plant, and early 1960s is found first in China Guangxi, is the rare plant resources in a kind of world.Camellia nitidissima is a kind of natural Chinese medicinal herb with high medical value, among the peoplely claim that again Camellia nitidissima is " a refreshing tea ", treat in drink, be a significant benefit to the health care of sub-health population as a kind of natural tea-drinking, residence, meet the Chinese Medicine theory, direction is controlled in the treatment that meets hypertension, high fat of blood, diabetes.Detect discovery through how tame authoritative mechanism, golden camellia tea contains multiple physiologically active ingredients such as tea polysaccharide, Tea Polyphenols, tea saponin, flavonoids, contains abundant germanium, selenium and zinc etc. simultaneously and keeps the health beneficial trace elements.Animal and clinical trial show that golden camellia tea has inhibitory action to the transplantability malignant tumour, also have hypotensive, reducing blood lipid and prevent effects such as atherosclerotic, along with people to the deepening continuously of Camellia nitidissima research, the high activity composition of Camellia nitidissima and the potentiality of the medicinal aspect of medical science are familiar with by common people gradually.
Round Camellia nitidissima in pharmaceutically application, people have carried out many effective researchs and exploration to Camellia nitidissima and extract thereof at present, the for example Chen Quanbin of Guangxi Normal University, profound will China, Zhang Qiaoyun, Liao Nazai " Guangxi tropical agriculture " 2005 (6) .-10-11, deliver the article of autograph for " separation of glycosides million is purified and sign in the golden camellia tea ", with the golden camellia tea is that raw material extracts flavones, flavones is through hydrolysis, and means such as solvent extraction, column chromatography obtain high-purity glucoside unit; Carry out structural characterization through analysis means such as fusing point, TLC, liquid chromatogram, infrared spectrum, nuclear magnetic resonance methods, confirm that first golden camellia tea contains glycosides displayed, its glucoside unit is Quercetin and Kaempferol.The Wei Lu of Guangdong Ocean University and Guangxi Fuxin Science ﹠ Technology Co., Ltd., Qin Xiaoming, Huang Riqiu, Huang Yingyi, Liu Zhixin is at " food science and technology " .2007,32 (11) .-100-102 have delivered " ultrasonic wave extracts the technical study of camellia chrysantha polysaccharide " this article and by single factor and orthogonal experiment the technology that ultrasonic wave extracts camellia chrysantha polysaccharide have been studied, inquired into solid-liquid ratio, extract temperature, these 4 influence factors of extraction time and ultrasonic frequency, the optimum extraction process condition of having determined camellia chrysantha polysaccharide is solid-liquid ratio 1: 50,80 ℃ of temperature, time 1.0h, ultrasonic frequency is 53.2kHz, and the yield of polysaccharide is 3.1% under this condition.Simultaneously supercritical ultrasonics technology and traditional extraction are compared, the result shows the yield 1.0% that adopts ultrasonic extraction to improve tea polysaccharide.
Aspect Camellia nitidissima extraction and making health food, we also retrieve following open source literatures, for example:
1, Chinese patent application number: 03149225.8, the applying date: 2003.06.18, title: a kind of Camellia nitidissima concentrate, open (bulletin) number: CN1460438, application (patent right) people: Guangxi Fuxin Science ﹠ Technology Co., Ltd., the address: Beihai Road ,Beihai City ,Guangxi Zhuang Autonomousnationality District panorama mansion east seat the 8th buildings, summary: this disclosure of the Invention a kind of Camellia nitidissima concentrate.All adopted conventional high temperature to extract method for concentration to concentrating of Camellia nitidissima extract at present, under the condition of high temperature, the aromatic substance volatilization in the Camellia nitidissima has been scattered and disappeared, active component is subjected to than havoc.What the present invention adopted is that nanometer film is separated concentration technique, under 25-40 ℃ of condition the Camellia nitidissima extract is concentrated, and has avoided the destruction of heating concentration process to active component, and the loss of active ingredient.The present invention is the basis of carrying out the Camellia nitidissima series product development, can further develop Camellia nitidissima food, beverage, health products, commodity and medicine.
2, Chinese patent application number: 03140885.0, title: a kind of Camellia nitidissima extract, open (bulletin) number: CN1476767, application (patent right) people: Guangxi Fuxin Science ﹠ Technology Co., Ltd., address: seat the 8th buildings, Beihai Road ,Beihai City ,Guangxi Zhuang Autonomousnationality District panorama mansion east, summary: a kind of Camellia nitidissima extract.Contain many compositions in the Camellia nitidissima to the human body beneficial; but be not fully used for a long time; the method of existing extraction Camellia nitidissima composition is that high temperature extracts and concentrates; can destroy part active ingredient like this; the present invention adopts alcohol extracting and water to carry and combines; and employing supersonic oscillations; to improve extraction efficiency; overall process has adopted and has been lower than 60 ℃ cryogenic conditions; aromatic substance in the Camellia nitidissima and various compositions have effectively been protected with health care; more than the extraction rate reached to 90%, and can shorten extraction time, reduce cost.
3, research [author] Zhao Yanhua of [autograph] Processing Technology of Yellow Flower Camellia Beverage, Tian Chengrui, Xu Changbo, Wei energy, Qin Lihu.Department of Food Engineering of [mechanism] Shaanxi Normal University, the modern drink of Xi'an starfish Co., Ltd, Fangchenggang City Camellia nitidissima Co., Ltd, Xi-an Milk Products Science Inst..[periodical name] Food Science .2005,26 (9) .-323-326.[digest] this paper has studied the basic technology of camellia chrysantha beverage lixiviate under the working condition, and prevents that the clarification process of shelf life muddiness from appearring in camellia chrysantha beverage.By multifactor orthogonal experiment, determined the best production technology of camellia chrysantha beverage.
4, [autograph] oral honeysuckle flower tea Research on processing technology [author] Ning Enchuan, Qin Xiaoming, Yang Hong.[mechanism] Guangxi University light industry and food engineering institute, food science and technology institute of Marine University Of Zhanjiang, Guangxi Fuxin Science ﹠ Technology Co., Ltd..[periodical name] food industry science and technology .2006,27 (1) .-121-122,125.[digest] inquired into the processing technology and the optimum formula of oral honeysuckle flower tea, with the Camellia nitidissima is raw material, adopt enzymolysis processing, handle extraction golden camellia tea pharmaceutical components in conjunction with supersonic oscillations, filtered out the optimum formula of oral liquid by orthogonal experiment, developed a kind of Camellia nitidissima peculiar flavour that has, little hardship enters the mouth, long times of aftertaste, the tangible health product of hypolipemic function.
5, [autograph] golden camellia tea pharmaceutical components novel technology for extracting research [author] Qin Xiaoming, Ning Enchuan, Yang Hong.Food science and technology institute of [mechanism] Marine University Of Zhanjiang, Guangxi University's light industry and food engineering institute, Guangxi Fuxin Science ﹠ Technology Co., Ltd..[printing name] food industry science and technology .2005,26 (10) .-122-124[digests] purpose: inquire into and adopt enzymolysis processing in conjunction with the action effect of supersonic oscillations processing to golden camellia tea pharmaceutical components leaching rate.Method: as leaching index,, determine from golden camellia tea, to extract the optimum extraction process condition of pharmaceutical components by orthogonal experiment with Tea Polyphenols and total saponin.The result: best of breed is that ultrasonic frequency is 25kHz, extracts 85 ℃ of temperature, extraction time 90min; The actual effect of middle trial production shows.New technology is compared with existing production technology, and the extraction rate of Tea Polyphenols, general flavone and total saponin has improved 17.3%, 13.2% and 9.3% respectively, and the extracting activity time has shortened 2h.
6, [autograph] Camellia nitidissima concentrating drinking liquid Research on processing technology [author] Yang Hong, Qin Xiaoming, Ning Enchuan.[mechanism] Guangxi Fuxin Science ﹠ Technology Co., Ltd., Marine University Of Zhanjiang, Guangxi University.[periodical name] Guangxi tropical agriculture .2005 (3) .-38-39[digest] adopt enzymolysis processing to handle extraction golden camellia tea pharmaceutical components in conjunction with supersonic oscillations, filter out the optimum formula of concentrating drinking liquid by orthogonal test, development has the health product of Camellia nitidissima peculiar flavour.
7, research [author] Wang Yuanfeng, the Wang Dengliang etc. of [autograph] golden camellia tea Enzymatic Extraction process conditions.[mechanism] Southern Yangtze University Foodstuffs Academy, Agricultural University Of South China.[periodical name] Wuxi Light Industry Univ.'s journal: food and biotechnology .2001,20 (6) .-582-587, the 593[digest] add exogenous enzymes the extracts active ingredients in the golden camellia tea is come out, its optimum extraction condition is: amount of water is 100 times of golden camellia tea dry sample, the mass fraction of the papain that adds is 0.4%, the pH value is 5.0-5.5, and temperature is 50-55 ℃, constant temperature 120min.With this understanding, golden camellia tea water leaching rate, soluble sugar and amino acid content are compared respectively according to increasing by 39.47%, 7.39% and 1.84%, the amino acid whose total leaching rate of crude protein is about 25.5%, and the leaching rate of mineral element Fe, Zn, Se, Mn, Co, Mo, Ge, V is all more than 95% in the golden camellia tea.
Recognize from above-mentioned open source literature, composition Study and the extraction of Camellia nitidissima at present, the health product of producing is more, but because several respects shortcoming is arranged with the active ingredient of commonsense method extraction golden camellia tea, the one, Camellia nitidissima blade wax coat is extremely thick, active component is difficult to transfer in the extract, and the 2nd, the easy oxidation stain of product.Though above-mentioned document discloses the technology of ultrasonic wave extraction Camellia nitidissima active component, but the past concentrates the general vacuum that adopts of concentrating of Camellia nitidissima active component, heat time heating time is long, so the rate of recovery of Camellia nitidissima active component and activity are lower, and the effect of making product also decreases.
Anti-oxidant, improve aspect the body immunity class health products, finding is many in the market plants or the plurality of Chinese plant is that raw material extract and are made with single, product form mainly contains health care wine, oral liquid, capsule and electuary, a lot of rules of origin are in ginseng class Chinese medicine.We can say that material source is more single.It should be noted that in addition, present most health products only rest on the animal efficacy test, for efficacy factor not further investigation still, product specification is lower, therefore be difficult to reach the requirement of third generation health food and integrate with world's health-product market, serious restriction the deep development of Chinese health products.
Summary of the invention
The purpose of this invention is to provide a kind of saponin class material that extracts from the plant golden camellia tea, and be made into soft capsule, and the production method of this soft capsule.
Soft capsule of camellia chrysantha tea of the present invention comprises the raw material of following composition and mass fraction:
Camellia nitidissima saponin (saponin powder) 40-60 part;
Vegetable oil 40-60 part;
Beeswax 0.2-1.0 part.
Above-described Camellia nitidissima saponin (saponin powder) is the active principle that extracts from the fresh blade of Camellia nitidissima.
Above-described vegetable oil comprises wherein one or more the mixing of tea-seed oil, rapeseed oil, peanut oil, palm oil or olive oil.
Above-described beeswax is to obtain material from honeycomb through processing.
Described Camellia nitidissima saponin is the material that obtains with following extracting method:
(1) raw material is handled
The fresh blade of Camellia nitidissima that harvesting is no more than 24 hours is removed yellow leaf and impurity, clean, be broken into the broken blade of strip about 1cm.
(2) lixiviate: Camellia nitidissima fresh leaf fragment adds clear water, adopt ultrasonic wave extraction or ultrasonic wave extraction in conjunction with enzymolysis processing, wherein the ultrasonic wave extraction is than 1: 10 at Camellia nitidissima fresh leaf fragment and clear water quality, extraction temperature 60-80 ℃, extraction time 60-70 minute, extract under the frequency 25-80kHz condition;
Described ultrasonic wave extraction is that the Camellia nitidissima blade is moved into the ultrasonic wave extractor in conjunction with enzymolysis, and the pure water that adds 5 times stirs, and is heated to 40 ℃, adds the compound pulp enzyme of reduction of feed volume 0.05% then, and constant temperature kept 2 hours, and constantly stirred.After finishing, enzymolysis processing is heated to 100 ℃ of enzymes 10 minutes of going out rapidly.Add 5 times of pure water of bright leaf weight again, when slurry temperature reaches the 60-70 ℃ of left and right sides, by ultrasonic wave traditional Chinese medicine extraction unit (TCD-1000) to the extraction of vibrating of the saponin active component in the bright leaf of Camellia nitidissima.For the first time supersonic oscillations finish the back and filter, and residue adds 10 times pure water again to carry out second time supersonic oscillations and extract (extraction conditions is with the first time).
(3) filter: leaching liquor is incorporated into stainless steel storage tank after 120 purpose economic benefits and social benefits filters filter stand-by;
(4) NF membrane is separated concentrated: above-mentioned solution filtration back is concentrated under 40-60 ℃ condition, adopt the pressurization nano filtering process to concentrate and produce the Camellia nitidissima concentrate, nanofiltration membrane component is the product of U.S. GE company, OSMONIC or KOCH company, and model is a DK series, effective area 2.5m
2, the material polyamide also can use cellulose acetate film; A whole set of experimental provision is cleaned three parts and is formed by preliminary treatment, nanofiltration, and material is pressurizeed through force (forcing) pump by Raw material pail, operating pressure 1.5Mpa sends into nanofiltration membrane component, regulates the NF membrane outlet valve, make filter pressure reach predetermined value, material is divided into filtered solution and concentrate after NF membrane is filtered.Filtered solution enters the clear liquid jar, and concentrate is got back to concentration tank after assembly flows out, and so constantly circulation realizes concentrating of feed liquid and separate that the ultimate density index is a standard with solid content 8-10%.
(5) Camellia nitidissima saponin purifying
Adopt Diaion HP-10 macroporous absorbent resins such as (Mitsubishi compound probability companies) to make separation and purification Camellia nitidissima saponin contrast test, select best absorbent resin and technical data.Macroporous absorbent resin is loaded in the glass cylinder, and fully wash chromatographic column with distilled water, NF membrane is separated the solution that concentrates per hour press the speed process resin column that 50-100 rises, use mass concentration 20-80% ethanolic solution wash-out then, obtain the Camellia nitidissima saponin (regeneration of resin was soaked 5-10 hour with alcohol 95 %) of purifying, and carry out ethanol and reclaim.
(6) spray-drying
Adopt spray-dired technology to carry out drying above-mentioned concentrate, import wind-warm syndrome degree is 170-180 ℃; Outlet wind-warm syndrome degree is 90-95 ℃.The Camellia nitidissima saponin powder of spray-drying gained is light yellow even powdered granule, and moisture content is 3.1%.
The production method of soft capsule of camellia chrysantha tea of the present invention:
Get spray-dired Camellia nitidissima saponin fine powder, vegetable oil, beeswax by making suspended matter at 1: 1: 0.02, with gelatin: glycerine: water is that 1: 0.35: 0.9 ratio prepares rubber, then the suspended matter can is pressed into soft capsule, typing below 25 ℃, with ethanol flush away soft capsule appearance oil reservoir, in dry below 25 ℃, take out, promptly.
Advantage of the present invention:
1, the composition of Camellia nitidissima saponin mainly is Quercetin and Kaempferol.A large amount of medical clinical test results show, that Camellia nitidissima has is hypoglycemic, hypotensive, fall cholesterol in serum, suppress tumor growth, prevent atherosclerotic, the human activin plurality of enzymes, improve body immunity, anti-oxidant, effect such as delay senility.According to the constituent analysis result of Camellia nitidissima, many experts infer that these effects of Camellia nitidissima and saponin class chemical composition have closely related.
2, adopt low-temperature ultrasonic to extract golden camellia tea, compared, because disclosed golden camellia tea extracting technology is to continue to use traditional workshop-based Chinese herbal medicine decoction method promptly to adopt jacketed pan high temperature to extract the constant-pressure and high-temperature concentration technology with former golden camellia tea extracting technology.Adopt the product of this explained hereafter, the partly or completely forfeiture of the physiological activator of health care, the most of volatilization loss of distinctive aromatic substance; The recovery rate of medicinal health composition is low, causes unit product raw material (bright leaf) consumption big, institute's product processed (weak flavor has the excitant peculiar smell) of low grade, and quality is very unstable.And the present invention adopts the low-temperature ultrasonic extractive technique that the saponin component in the Camellia nitidissima is extracted separation, can reduce energy consumption, shorten extraction time, reduce possible destruction in the leaching process, effectively improve the rate of recovery and active maintenance of Camellia nitidissima active component, saponin powder purity reaches more than 90%.
3, adopt macroporous absorbent resin high-efficiency adsorbent separation and purification Camellia nitidissima saponin, it is good to have selectivity, and the characteristics that separative efficiency is high have effectively improved the rate of recovery of Camellia nitidissima saponin component, and activity can keep preferably, and is higher more than 30% than ethanol precipitation.
4, soft capsule of camellia chrysantha tea holding time of obtaining of production of the present invention long, the active component content height.Products such as our oral honeysuckle flower tea of once developing of past, Camellia nitidissima instant tea, camellia chrysantha beverage are not because efficacy factor is separated bright, these products also only rest on the primary product stage, product specification also is difficult to promote, and does not catch up with the requirement of " third generation health products " health products.So the present invention is exploitation efficacy factor clear and definite novel product in breach with the soft capsule of camellia chrysantha tea, improve the technology content and the class of product, promote the potentiality advantage of enterprise development, and in intense market competition, try to achieve and develop.
5, the present invention considers that also the medicine dissolubility well might not the bioavilability height, therefore in soft capsule of camellia chrysantha tea, add vegetable oil, beeswax,, make the quick stripping of Camellia nitidissima saponin and see through biomembrane to improve the diffusion of mucous membrane rete malpighii between cell membrane, release fast increases absorption.
6, by deep processing to Camellia nitidissima; adopt new and high technology; implement the strategy of three high low (high-tech, high-quality, high-quality service, low costs); agricultural byproducts with low value are produced high value-added product; make the agricultural product increment; reach increasing peasant income; enterprise makes a profit; increase state revenue and expenditure; simultaneously can also improve the understanding of people to the health-care effect of Camellia nitidissima; reinforcement solves a part of surplus labor's the problem of employment to this rare plant resources effective protection of Camellia nitidissima, embodies good social benefit.The present invention also can develop the economic worth of Camellia nitidissima and the formation industry, promotes the Camellia nitidissima value-added content of product, and the Camellia nitidissima raw material is rationally utilized.
7, economic benefit of the present invention, production cost: the soft capsule of camellia chrysantha tea product that average every production is 1 ton, need: 5 tons of Camellia nitidissima fresh leafs are worth 200,000 yuan, 1 ton of pure water, be worth 0.02 ten thousand yuan, the auxiliary material that needs takes 80,000 yuan in addition, and packaging material take 140,000 yuan, 60,000 yuan of processing charges, 60,000 yuan of administration fees, add up to 550,000 yuan by other 0.98 ten thousand yuan.
8, the production marketing price is with reference to the wholesale price of existing market like product, and the price of project product soft capsule has the very strong market competitiveness with 0.35 yuan of/every bottle of calculating.Project normal year sales volume income is 5,430,000 yuan, 156.5 ten thousand yuan of annual profits tax.
The specific embodiment
The fresh blade of Camellia nitidissima that harvesting is no more than 24 hours is removed yellow leaf and impurity, clean, be broken into the broken blade of strip about 1cm, adopt the ultrasonic wave extraction then, Camellia nitidissima fresh leaf fragment and clear water quality were than 1: 10, extraction temperature 60-80 ℃, extraction time 1-2h, effective component extracting under the frequency 25-80kHz.The solution that then the ultrasonic wave lixiviate is obtained filters the back and concentrates under 40-60 ℃ condition, adopts nano filtering process to concentrate and produces the Camellia nitidissima concentrate; Operating pressure 1.5Mpa, filtered solution flow 1.75LPM, concentrated solution discharge 43LPM, the ultimate density index is with solid content 8-10%.Adopt Diaion HP-10 macroporous absorbent resins such as (Mitsubishi compound probability companies) to make separation and purification Camellia nitidissima saponin contrast test, select best absorbent resin and technical data.Macroporous absorbent resin is loaded in the glass cylinder, and fully wash chromatographic column with distilled water, NF membrane is separated the solution that concentrates per hour press the speed process resin column that 50-100 rises, ethanolic solution with 20-80% carries out wash-out then, obtain the Camellia nitidissima saponin (regeneration of resin was soaked 5-10 hour with alcohol 95 %) of purifying, and carry out ethanol and reclaim.Concentrate carries out spray-drying, and spray-drying import wind-warm syndrome degree is 170-180 ℃, and outlet wind-warm syndrome degree is 90-95 ℃.The Camellia nitidissima saponin powder of spray-drying gained is light yellow even powdered granule, and moisture content is 3.1%.Get spray-dired Camellia nitidissima saponin fine powder, vegetable oil, beeswax by making suspended matter at 1: 1: 0.02, with gelatin: glycerine: water is that 1: 0.35: 0.9 ratio prepares rubber, then the suspended matter can is pressed into soft capsule, typing below 25 ℃, with ethanol flush away soft capsule appearance oil reservoir,, take out in dry below 25 ℃, sampling inspection obtains the soft capsule of camellia chrysantha tea finished product.
The fresh blade of Camellia nitidissima that harvesting is no more than 24 hours is removed yellow leaf and impurity, clean, be broken into the broken blade of strip about 1cm, then the Camellia nitidissima blade is moved into the ultrasonic wave extractor, the pure water that adds 5 times stirs, be heated to 40 ℃, the compound pulp enzyme that adds reduction of feed volume 0.05% then, constant temperature kept 2 hours, and constantly stirred.After finishing, enzymolysis processing is heated to 100 ℃ of enzymes 10 minutes of going out rapidly.Add 5 times of pure water of bright leaf weight again, when slurry temperature reaches the 60-70 ℃ of left and right sides, by ultrasonic wave traditional Chinese medicine extraction unit (TCD-1000) to the extraction of vibrating of the saponin active component in the bright leaf of Camellia nitidissima.For the first time supersonic oscillations finish the back and filter, and residue adds 10 times pure water again to carry out second time supersonic oscillations and extract (extraction conditions is with the first time).The solution that then lixiviate is obtained filters the back and concentrates under 40-60 ℃ condition, adopt nano filtering process to concentrate and produce Camellia nitidissima concentrate, operating pressure 1.5Mpa, filtered solution flow 1.75LPM, concentrated solution discharge 43LPM, the ultimate density index is a standard with solid content 8-10%.Adopt Diaion HP-10 macroporous absorbent resins such as (Mitsubishi compound probability companies) to make separation and purification Camellia nitidissima saponin contrast test, select best absorbent resin and technical data.Macroporous absorbent resin is loaded in the glass cylinder, and fully wash chromatographic column with distilled water, NF membrane is separated the solution that concentrates per hour press the speed process resin column that 50-100 rises, ethanolic solution with 20-80% carries out wash-out then, obtain the Camellia nitidissima saponin (regeneration of resin was soaked 5-10 hour with alcohol 95 %) of purifying, and carry out ethanol and reclaim.Concentrate carries out spray-drying, and spray-drying import wind-warm syndrome degree is 170-180 ℃, and outlet wind-warm syndrome degree is 90-95 ℃.The Camellia nitidissima saponin powder of spray-drying gained is light yellow even powdered granule, with 60 kilograms in the Camellia nitidissima saponin powder of above-mentioned spray-drying gained, adds 0.5 part in tea-seed oil or rapeseed oil 40-60 kilogram, beeswax.By making suspended matter at 1: 1: 0.02,90-102 ℃ of drying, packing, sterilization, sampling inspection down, again with gelatin: glycerine: water is that 1: 0.35: 0.9 ratio prepares rubber, then the suspended matter can is pressed into soft capsule, typing below 25 ℃ is with ethanol flush away soft capsule appearance oil reservoir, in dry below 25 ℃, take out, sampling inspection obtains the soft capsule finished product.
With 60 kilograms in the Camellia nitidissima saponin powder of above-mentioned spray-drying gained, add 0.5 part in peanut oil or rapeseed oil 40-60 kilogram, beeswax.By making suspended matter at 1: 1: 0.02,90-102 ℃ of drying, packing, sterilization, sampling inspection down, again with gelatin: glycerine: water is that 1: 0.35: 0.9 ratio prepares rubber, then the suspended matter can is pressed into soft capsule, typing below 25 ℃ is with ethanol flush away soft capsule appearance oil reservoir, in dry below 25 ℃, take out, sampling inspection obtains the soft capsule finished product.
Description of drawings
Fig. 1 is the removing lab diagram of soft capsule of camellia chrysantha tea active ingredient of the present invention to hydroxyl radical free radical (OH).
Fig. 2 is that soft capsule of camellia chrysantha tea active ingredient of the present invention is to superoxide anion (O
2 -) the clearance test lab diagram.
Fig. 3 is that soft capsule of camellia chrysantha tea active ingredient of the present invention is to nitrite ion (NO
2 -) the removing lab diagram.
Fig. 4 is that soft capsule of camellia chrysantha tea active ingredient of the present invention is to H
2O
2The removing lab diagram.
Following experimental study is seen in concrete explanation.
Soft capsule of camellia chrysantha tea active ingredient of the present invention is removed the Natural Antioxidants experimental study of multiple free radical
The inventor has the effect that can remove free radical in order to confirm soft capsule of camellia chrysantha tea active ingredient (saponin); To OH, O2 -、NO
2 -, and H2O
2Carried out clearance test.
1 materials and methods
1.1 material
1.1.1 raw material:
The spray-dired Camellia nitidissima saponin fine powder of the embodiment of the invention 1 is provided by Guangdong Ocean University Biotechnology Experiment chamber.
1.1.2 main agents:
It is pure that absolute ethyl alcohol, hydrochloride naphthodiamide, sulfanilic acid, natrium nitrosum, citric acid, ferrous sulfate, pyrogallol, hydrogen peroxide, Phen, hydrochloric acid, sodium hydrogen phosphate, sodium dihydrogen phosphate, 3-hydroxymethyl aminomethane, ascorbic acid, vanillic aldehyde, panaxoside standard items are analysis.
1.1.3 key instrument and equipment:
The UV-9100 ultraviolet-uisible spectrophotometer, HH-4 digital display thermostat water bath, the BP210S electronic analytical balance, SHB-3 circulation ability of swimming is used vavuum pump more, RE-52AA rotary evaporator, thunder magnetic pHSJ-4A acidometer.
1.2 experimental technique
1.2.1 the preparation of Camellia nitidissima saponin
Adopt Diaion HP-10 macroporous absorbent resin that the thick saponin S of Camellia nitidissima is carried out separation and purification, use distilled water, 30%, 60% ethanolic solution to carry out wash-out successively, obtain S
1, S
2Two key components, they are respectively by 30%, 60% ethanolic solution wash-out, with S, S
1, S
2Be mixed with respectively that saponin concentration is followed successively by 1,2,3,4, the solution of 5mg/mL, their antioxidation activity studied, and with V with concentration
CDo contrast, saponin content adopts the vanillin-sulfuric acid colorimetric method to measure.
1.2.2 hydroxyl radical free radical (OH) is removed experiment
Adopt Fenton (Fenton) system Phen-Fe
2+Oxidizing process is measured, and gets the Phen of 1.5mL 1mM and puts into test tube respectively, adds the PBS of 4.5mL 100mM pH=7.4, adds 1mL 1mM FeSO behind the mixing
4Solution, mixing adds the certain density test liquid of 1mL respectively immediately, adds 1mL 0.1%H then
2O
2Start reaction, in 37 ℃ of insulation 60min, the 536nm place measures absorbance.The damage pipe is set simultaneously (to add 1mL distilled water and replaces sample liquid, 1mL0.1%H
2O
2Start reaction) and do not damage pipe (add 2mL distilled water and replace sample liquid and hydrogen peroxide), oppose than test with the Vc of same concentrations, wherein damage is managed and is not decreased pipe and returns to zero with PBS, and chemical feed pipe is not to add H with concentration
2O
2Chemical feed pipe zeroing.Be calculated as follows the clearance rate of hydroxyl radical free radical:
The clearance rate of OH (%)=(A
Dosing-A
Damage/ A
Do not decrease-A
Damage) * 100%
1.2.3 superoxide anion (O
2 -) clearance test
Adopt pyrogallol autoxidation system method to measure, get 4.5mLpH=8.2Tris-HCl cushioning liquid, add the certain density test liquid of 1mL respectively, the pyrogallol that adds 0.3ml 1mM behind 25 ℃ of insulation 20min starts reaction, measure the absorbance A at 325nm place behind the 5min, contrast (distilled water that adds 4.2mL replaces sample liquid) is set simultaneously, and control tube returns to zero with cushioning liquid, and chemical feed pipe returns to zero with the same concentrations sample liquid respectively.Be calculated as follows the clearance rate of superoxide anion:
O
2 -Clearance rate (%)=(A
Contrast-A
Dosing/ A
Contrast) * 100%
1.2.4 nitrite ion (NO
2 -) removing experiment
Adopt nitroso system sulfanilamide (SN) colorimetric method to measure, get the 1mL test liquid in the 10mL colorimetric cylinder, add the NaNO of 5 μ g/mL
2Standard liquid 0.5mL reacts 30min in 37 ℃ of waters bath with thermostatic control.Add 1mL0.4% sulfanilic acid solution after the taking-up immediately, mixing leaves standstill the hydrochloride naphthodiamide solution that adds 0.5mL0.2% behind the 5min, adds water to the 10mL scale, and mixing leaves standstill 15min, not add NaNO
2With the reagent of sample solution be blank, in 538nm place mensuration light absorption value.Pass through NaNO
2Calibration curve obtains corresponding N aNO
2Content.Be calculated as follows NO
2 -Clearance rate:
1.2.5 remove hydrogen peroxide (H
2O
2) experiment
Get the phosphate buffer 4.5mL of PH=7.4, add 0.05%H
2O
2Behind the 2mL, get the 1mL test liquid, recording its absorbance at the 248nm place after mixing is A
1, in the experiment not add the H of test liquid
2O
2Absorbance is A
0, not add H
2O
2The sample solution absorbance be A
2, be calculated as follows its mean value.
2 results and analysis
2.1 hydroxyl radical free radical (OH) is removed experiment
OH is the important activity oxygen radical that causes lipid peroxidation, nucleic acid fracture, protein and polysaccharide to decompose, and is active oxygen the most active in the body.Adopt and utilize the Fenton system to detect Camellia nitidissima saponin, V
CTo the removing effect of OH, experimental result is seen Figure of description Fig. 1.As can be seen from Figure 1, Camellia nitidissima saponin and V
COH all there is the elimination effect, and is dose-effect relationship, wherein S
1Removing effect and V
CQuite, be to reach the half clearance rate between 4～5mg/mL in concentration; After concentration is greater than 1mg/mL, S, S
2The removing effect to obviously be better than V
C, both reach the half clearance rate between 2～3mg/mL.When sample liquid concentration reaches 5mg/mL, S, S
1, V
CClearance rate reached more than 85% and S
2Clearance rate then reach 97.44%.The author finds in the research in early stage, only adding concentration under same system is the Camellia nitidissima water extract of 1mg crude drug/ml, the clearance rate of OH promptly reaches 98.21%, and this has illustrated the stronger material of antioxidation activity that also contains other in the golden camellia tea except saponin.
2.2 superoxide anion (O
2 -) clearance test
Pyrogallol is rapid autoxidation under alkali condition, produces O in the autoxidation process
2 -, O
2 -Quicken pyrogallol autoxidation speed, generate coloured intermediate product simultaneously, strong light absorption is arranged, because the autoxidation rate dependent is in O at 325nm
2 -Concentration, remove O
2 -Then suppress automatic oxidation reaction, stop the accumulation of intermediate product, tried thing removing O thereby estimate
2 -Ability.Camellia nitidissima saponin and V
CTo O
2 -Removing effect such as Figure of description Fig. 2, as shown in Figure 2, experiment in the given scope, S, S
1, S
2And V
CTo O
2 -All have certain scavenging action, but S, S
1, S
2The removing effect be starkly lower than V
CThough the three is to reach the half clearance rate between 3～4mg/mL in concentration, experiment the clearance rate during given Cmax 5mg/mL only be 60% effect, wherein S, S
1Having occurred the negative of clearance rate during for 1mg/mL in concentration, may be to connect hydroxyl structure, O because they contain
2 -The autoxidizable while of pyrogallol is also quickened their autoxidation in the acceleration system, thereby produces more O
2 -, detection is negative scavenging action.But along with the increase of concentration, S, S
1Suppress O
2 -Effect is greater than O in the system
2 -Formation speed, clearance rate present on the occasion of.By finding that with the contrast of early-stage Study adding concentration under identical system only is the Camellia nitidissima water extract of 1mg crude drug/ml, O
2 -Clearance rate promptly reached 76.92%, this antioxidation that shows Camellia nitidissima once more produces by multiple one-tenth branch is collaborative.
2.3 nitrite ion (NO
2 -) removing experiment
The N-nitroso compound is the organic matter that a class has nitroso (N-NO) structure, and major part has carcinogenicity, can be synthetic in vivo and in vitro by its precursor nitrite and amine, and they are precarcinogen, need just have carcinogenicity through after the metabolism in vivo.Therefore, research can remove nitrite, suppress the effective way that the synthetic antioxidant of nitrosamine is the harm of prevention nitroso compound.The method of pressing 1.2.4 detects Camellia nitidissima saponin and V
CTo NO
2 -Scavenging action, experimental result is seen Figure of description Fig. 3, as shown in Figure 3, the Camellia nitidissima saponin all has certain scavenging action to nitrite, but the removing ability is obviously not as V
C, under the designed concentration of experiment, S, S
1, S
2To NO
2 -Scavenging action suitable, and, when concentration reaches 5mg/mL, just reached the half clearance rate, and the concentration of Vc is when being 1mg/mL along with its clearance rate of increase of concentration all presents ascendant trend slowly, clearance rate can reach 93.38%.
2.4H
2O
2Removing experiment
H
2O
2Be added into to decompose in the food and emit oxygen, play on the one hand effects such as bleaching, anticorrosion and deodorizing, can form epoxides with starch in the food on the other hand and cause the generation of alimentary tract cancer, therefore research can be decomposed the security that the antioxidant that remains in the hydrogen peroxide in the food can effectively improve food.Adopt method research Camellia nitidissima saponin and the V of 1.2.5
CTo H
2O
2Scavenging action, result such as Figure of description Fig. 4, the result as shown in Figure 4, S, S
1, S
2To H
2O
2All have certain scavenging action, and the removing ability is suitable in designed concentration range, clearance rate is all between 35%～52%, and concentration and its inhibiting rate be not tangible linear relationship, and experiment does not detect V
CTo H
2O
2Has scavenging action.
3 conclusions
Soft capsule of camellia chrysantha tea (Camellia nitidissima saponin) is to OH, O
2 -, NO
2 -, and H
2O
2All has scavenging action, though to O
2 -, NO
2 -Scavenging action not as good as V
C, but to OH and H
2O
2The removing effect but obviously be better than V
C, especially outstanding to the scavenging action of OH, experimental result proof Camellia nitidissima saponin is a kind of natural anti-oxidation material that can remove multiple free radical; Experiment is also found, different Camellia nitidissima saponin components also have difference in identical concentration and the scavenging action under the free radical system, this structure with them is relevant closely, and further separation and purification, the structural analysis of therefore relevant Camellia nitidissima saponin are still waiting more deep research; In addition, by finding that with the contrast of early-stage Study the antioxidation activity of Camellia nitidissima is by its saponin class and the synergistic result of other active components.So the saponin class material that the antioxidation of soft capsule of camellia chrysantha tea contains with it is closely related, and result of the present invention provides theoretical foundation for the functional food that the Camellia nitidissima exploitation is become aspects such as anticancer, anti-ageing and cardiovascular protection.
The edible case history of soft capsule of camellia chrysantha tea of the present invention:
Example 1, Lee * *, the man, 45 years old, people from Qinzhou City, Guangxi, the real estate boss because of gluttony, suffers from obesity and coronary heart disease, uncomfortable in chestly breathes hard, often feels unable, off color.Take soft capsule of camellia chrysantha tea of the present invention, every day three times, each 2, after 3 months, lost weight, only surplus slightly breathing hard and dizzy symptom, surplus disease disappears, and the state of mind might as well.
Example 2, yellow * *, the woman, 50 years old, people from Zhanjiang City, Guangdong, the worker of enterprise, because busy work all the year round, have no time to attend to and take good care of one's health so that fall sick from overwork, immunity degradation, feel that health is tired, sit down and just do not remember, that inefficiency, energy plentifully, are not upstairs panted is unable, easy catching a cold, decrease of memory, distraction, face gloomy unglazed, be full of wrinkles, skin does roughly, lives the low quality life.Take soft capsule of camellia chrysantha tea of the present invention, every day three times, each 2, after 2 months, skin begins smooth high resilience, and sleep also improves.
Example 3, Zhao * *, the man, life in 1962, Nanning people from city, because of suffering from high fat of blood, concurrent hypertension, coronary heart disease, also often dizzy, asthma upstairs, energy is not abundant, dizziness.In certain hospitalize, take the xx medicine, but symptom makes moderate progress at the beginning of 2008, but the symptom commentaries on classics of not getting better after the drug withdrawal, after change and take soft capsule of camellia chrysantha tea of the present invention, every day three times, each 2, take after 20 days and take a turn for the better to some extent, take symptom part disappearance spirit improvement after month, continue to take two weeks, all illness disappears, of pink and healthy-looking, to feel good, dizzy symptom might as well.
Example 4, open * *, the man, nineteen fifty-three gives birth to, people from Beihai, Guangxi often labors for breath, fatiguability, on June 10th, 2007 behind examination in hospital, also found to suffer from coronary heart disease, but be not in hospital owing to lack of capital, take soft capsule of camellia chrysantha tea of the present invention, every day 3-4 time, each 2, take the aftersensation in February and get that sb.'s illness took a favorable turn, breathe smooth and easyly, spirit might as well.
Claims (7)
1, a kind of soft capsule of camellia chrysantha tea is characterized in that: its primary raw material comprises the composition of following mass fraction:
Camellia nitidissima saponin 40-60 part;
Vegetable oil 40-60 part;
Beeswax 0.2-1.0 part.
2, soft capsule of camellia chrysantha tea according to claim 1 is characterized in that: described vegetable oil comprises wherein one or more the mixing of tea-seed oil, rapeseed oil, peanut oil, palm oil or olive oil.
3, soft capsule of camellia chrysantha tea according to claim 1 is characterized in that: described beeswax is to obtain material from honeycomb through processing.
4, soft capsule of camellia chrysantha tea according to claim 1 is characterized in that: described Camellia nitidissima saponin is the material that obtains with following extracting method:
(1) raw material is handled: the fresh blade of Camellia nitidissima that harvesting is no more than 24 hours is removed yellow leaf and impurity, clean, be broken into the broken blade of strip about 1cm;
(2) lixiviate: Camellia nitidissima fresh leaf fragment adds clear water, adopts ultrasonic wave extraction or ultrasonic wave extraction to obtain leaching liquor in conjunction with enzymolysis processing;
(3) filter: leaching liquor is incorporated into stainless steel storage tank after 120 order economic benefits and social benefits filters filter standby;
(4) NF membrane is separated concentrated: adopt the pressurization nano filtering process to concentrate filtered fluid and produce the Camellia nitidissima concentrate, material is pressurizeed through force (forcing) pump by Raw material pail, operating pressure is 1.5Mpa, send into nanofiltration membrane component, regulate the NF membrane outlet valve, make filter pressure reach predetermined value, material is divided into filtered solution and concentrate after NF membrane is filtered, filtered solution enters the clear liquid jar, concentrate is got back to concentration tank after assembly flows out, so constantly circulation realizes concentrating of feed liquid and separates filtered solution flow 1.75LPM, concentrated solution discharge 43LPM;
(5) Camellia nitidissima saponin purifying: macroporous absorbent resin is loaded in the glass cylinder, NF membrane is separated the solution that concentrates per hour press the speed process resin column that 50-100 rises, use mass concentration 20-80% ethanolic solution wash-out then, obtain the Camellia nitidissima saponin of purifying, regeneration of resin is with 95% alcohol immersion 5-10 hour, and carries out ethanol and reclaim;
(6) spray-drying: adopt spray-dired technology to carry out drying above-mentioned concentrate, import wind-warm syndrome degree is 170-180 ℃; Outlet wind-warm syndrome degree is 90-95 ℃, and the Camellia nitidissima saponin powder of spray-drying gained is light yellow even powdered granule, and moisture content is 3.1%.
5, soft capsule of camellia chrysantha tea according to claim 4, it is characterized in that: described ultrasonic wave extraction is than 1: 10 at Camellia nitidissima fresh leaf fragment and clear water quality, extraction temperature 60-80 ℃, extraction time 60-70 minute, extract under the frequency 25-80kHz condition.
6, soft capsule of camellia chrysantha tea according to claim 4, it is characterized in that: described ultrasonic wave extraction is that the Camellia nitidissima blade is moved into the ultrasonic wave extractor in conjunction with enzymolysis, the pure water that adds 5 times stirs, be heated to 40 ℃, the compound pulp enzyme that adds reduction of feed volume 0.05% then, constant temperature kept 2 hours, and constantly stirred.Be heated to 100 ℃ of enzymes 10 minutes of going out after enzymolysis processing finishes rapidly, add 5 times of pure water of bright leaf weight again, when slurry temperature reaches the 60-70 ℃ of left and right sides, by ultrasonic wave traditional Chinese medicine extraction unit to the extraction of vibrating of the saponin active component in the bright leaf of Camellia nitidissima; For the first time supersonic oscillations finish the back and filter, and residue adds 10 times pure water again to carry out second time supersonic oscillations and extract, and extraction conditions is with the first time.
7, the production method of soft capsule of camellia chrysantha tea as claimed in claim 1, it is characterized in that: get spray-dired Camellia nitidissima saponin fine powder, vegetable oil, beeswax by making suspended matter at 1: 1: 0.02, with gelatin: glycerine: water is that 1: 0.35: 0.9 ratio prepares rubber, then the suspended matter can is pressed into soft capsule, typing below 25 ℃ is with ethanol flush away soft capsule appearance oil reservoir, in dry below 25 ℃, take out, promptly.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103141853A (en) * | 2013-03-08 | 2013-06-12 | 中华全国供销合作总社杭州茶叶研究所 | Theaflavin health-care food or medicament and preparation method thereof |
| CN107753451A (en) * | 2017-11-28 | 2018-03-06 | 李妍 | A kind of preparation method for treating halitosis lozenge |
| CN111838370A (en) * | 2020-07-29 | 2020-10-30 | 周丽生 | Tamarind leaf medicinal tea with effects of regulating spleen and stomach, clearing heat and expelling toxin and production process thereof |
-
2009
- 2009-05-08 CN CNA2009101140408A patent/CN101558808A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103141853A (en) * | 2013-03-08 | 2013-06-12 | 中华全国供销合作总社杭州茶叶研究所 | Theaflavin health-care food or medicament and preparation method thereof |
| CN107753451A (en) * | 2017-11-28 | 2018-03-06 | 李妍 | A kind of preparation method for treating halitosis lozenge |
| CN111838370A (en) * | 2020-07-29 | 2020-10-30 | 周丽生 | Tamarind leaf medicinal tea with effects of regulating spleen and stomach, clearing heat and expelling toxin and production process thereof |
| CN111838370B (en) * | 2020-07-29 | 2023-02-03 | 周丽生 | Tamarind leaf medicinal tea with effects of regulating spleen and stomach, clearing heat and expelling toxin and production process thereof |
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Application publication date: 20091021 |