CN103908523B - Method for extracting tea pigment from tea leaves and tea pigment soft capsule - Google Patents

Method for extracting tea pigment from tea leaves and tea pigment soft capsule Download PDF

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CN103908523B
CN103908523B CN201410176092.9A CN201410176092A CN103908523B CN 103908523 B CN103908523 B CN 103908523B CN 201410176092 A CN201410176092 A CN 201410176092A CN 103908523 B CN103908523 B CN 103908523B
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tea
pigment
content
tea pigment
oil
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CN103908523A (en
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刘志炯
许效鸿
王祖海
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CHONGQING HAILIYUN TECHNOLOGY Co Ltd
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CHONGQING HAILIYUN TECHNOLOGY Co Ltd
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Abstract

The invention discloses a method for extracting tea pigment from tea. The method is characterized by including the following steps: (1) rubbing tea leaves into 20-40 mesh mash, and standing for 1-4 hours; (2) performing continuous countercurrent extraction on the mash by hot water with temperature being higher than 80 DEG C; (3) filtering the extracting solution by using 80-mesh screen cloth, performing microfiltration, ultrafiltration and nanofiltration concentration until the density of the extracting solution is 1.15-1.2 g/cm<3>, performing vacuum concentration until the density of the extracting solution is 1.3g/cm<3>, and spray drying and crushing to obtain a product. The invention further discloses a tea pigment soft capsule, composed of contents and a capsule material, wherein the contents are tea pigment extracted in claim 1 and edible vegetable oil, and the weight ratio of the tea pigment to the edible vegetable oil is 1:(2-4); the capsule material is prepared from gelatin, glycerin, pure water and natural edible pigment according to a ratio being (38-39):(11-12):(49-50):(0.25-0.3) in parts by weight. The extraction method disclosed by the invention is energy-saving, low in cost and environmental-friendly, and the content of the obtained product tea pigment is high. The properties of the prepared soft capsule are stable.

Description

The method and dark brown cellulose soft capsules of Tea Pigment are extracted from tealeaves
Technical field
The present invention relates to a kind of method that Tea Pigment is extracted from tealeaves, the invention further relates to a kind of dark brown cellulose soft capsules.
Background technology
Tea Pigment is the class day that catechin is polymerized through enzyme/non-enzymatic oxidative dehydrogenation in pairs in fresh tea passes or green tea Right high bioactivity compound, its main component is tea uranidin class, tea red pigment class and dark brown pigment Polyphenols and its spreads out Biological mixture.Tea Pigment has very strong anti-oxidant and elimination free radical ability, wherein theaflavin and thearubigin activity most By force, the medicine materials such as preventing and treating cardiovascular and cerebrovascular disease, atherosclerosis, reducing blood lipid and hypotensive are now had been used to, its outward appearance is Yellowish red is relatively soluble in alcohol, ethyl acetate to peony amorphous powder, can be soluble in water.At present, extracted from tealeaves The method of Tea Pigment has solvent extraction, solvent extraction+alkaline oxygenated method and solvent extraction+acidic oxidation method.
As Chinese patent application 200610016250.X discloses a kind of Chinese medicine preparation of reducing blood pressure and regulating blood lipid, the effective portion of tealeaves is extracted The method divided is to rub tealeaves with the hands broken, and with 2-8 times of ethanol heating and refluxing extraction, ethanol is reclaimed in then vacuum distillation, is concentrated into every Milliliter contained 0.5g etc..And for example Chinese patent CN1031309C discloses a kind of extracting method of Tea Pigment, and flow is:Leaching Bubble concentration-chemical extraction-tune pH- suction filtrations-separation and Extraction-drying, wherein chemical extraction are add three-to-four-fold 95% ethanol Extracted, it is to be hydrogenated with sodium oxide molybdena so that pH is adjusted to 7.0-7.5 to adjust pH so that catechin is aoxidized, and separation-extraction technology adds three Chloromethanes.The method uses poisonous chloroform, is likely to result in noxious material residual, is that modern food medicine is difficult to receive.
Chinese patent application CN102675906A discloses a kind of extracting method of tea red pigment, with tea powder as raw material, side The stirring of heating side, 90-95 degree is heated to tea ash aqueous, is incubated 5-15 minutes, then pours out millet paste, and hydroxide is then used again Sodium adjusts PH so that between 9-10, heating-up temperature carries out air oxidation 4-5h, most to PH at this temperature below 80 degrees Celsius Rufous concentration crude product is obtained afterwards.40-60 parts of ethanol is added in the concentration crude product again, stirring stands filtering, and filter cake is through dry It is dry to obtain product.The above method is organic solvent+alkaline oxygenated method.
Above two method is by alkaline oxygenated so that catechin is oxidized to Tea Pigment, and alkaline oxygenated product is complicated, In the presence of many unknown materials, dark brown cellulose content is relatively low, and its health-care effect is poor.
Soft capsule has circle also known as flexible glue pill, its shape, oval, fish shape, tubular etc..It is by oils or to bright Glue thing water-insoluble liquid or suspension without dissolution etc. are closed in a kind of preparation in capsule shells.At present, tea Pigment is also not used for being made soft capsule.
The content of the invention
The technical problems to be solved by the invention be provide a kind of energy-conservation, low cost, dark brown cellulose content it is high, environmentally friendly from The method that tea red pigment is extracted in tealeaves, the method is not use any organic solvent, acid solution and alkali lye, using fresh tea passes in itself The polyphenol oxidase being had(PPO)And peroxidase(POD)Oxidation polymerization under certain condition produces Tea Pigment, is environment Friendly technique.Another object of the present invention is to the Tea Pigment of extraction is made into soft capsule, good stability.
What the first object of the present invention was realized in:A kind of method that Tea Pigment is extracted from tealeaves, it is characterised in that: Extract in accordance with the following steps:
(1), will not rub into 20-40 mesh pastel by the tealeaves of de-enzyme treatment, place 1-4h;
(2), with temperature Continuous Countercurrent Extraction is carried out to above-mentioned pastel more than 80 DEG C of hot water;
(3), by extract solution with 80 mesh sieve net filtrations, being then concentrated into extract solution density through micro-filtration, ultrafiltration, nanofiltration is 1.15-1.2 g/cm3, extract solution density is then concentrated in vacuo to again for 1.3g/cm3, then obtain product by spray drying.
As preferred:Step(1)In, fresh tea passes are rubbed with stainless steel meat grinder.Step(3)In, it is desirable to it is crushed to 100 Below mesh.Products obtained therefrom includes theaflavin, thearubigin and theabrownin, and the total amount of the theaflavin, thearubigin and theabrownin is more than 65%, the wherein content of thearubigin is more than or equal to 22%, and theaflavin content is more than or equal to 13%, and dark brown pigment content is more than or equal to 30%。
Using said extracted method:First:We, as raw material, tealeaves are twisted using not by the tealeaves of de-enzyme treatment It is broken, place at room temperature, without any acid solution and alkali lye, the natural polyphenol oxidizing ferment contained using tealeaves(PPO)And mistake Oxide enzyme(POD)Catechin in tealeaves is oxidized to theaflavin, thearubigin.So as to theaflavin, thearubigin and tea in product The content of brown element is high.If tealeaves is processed by de-enzyme, will no longer contain polyphenol oxidase and peroxidase.Secondly, this hair It is bright that nanofiltration concentration, energy-conservation, water saving were first passed through before vacuum concentration.
It is another object of the present invention to what is be achieved in that:A kind of dark brown cellulose soft capsules, are made up of content and capsule material, described Content is the Tea Pigment and edible vegetable oil that claim 1 is extracted, and the Tea Pigment is 1 with the weight ratio of edible vegetable oil: 2-4;The capsule material is gelatin by according to ratio of weight and number:Glycerine:Pure water:Natural food colour=38-39:11-12:49-50: The raw material of 0.25-0.3 are obtained.
In the above-mentioned technical solutions:The Tea Pigment includes theaflavin, thearubigin and theabrownin, the theaflavin, congo red The total amount of element and theabrownin is more than 65%, and the wherein content of thearubigin is more than or equal to 22%, and theaflavin content is more than or equal to 13%, tea Brown cellulose content is more than or equal to 30%.
In the above-mentioned technical solutions:The preparation method of dark brown cellulose soft capsules is:
A. the preparation of capsule material:
(1), in gelatin add portion of pure water expand it;Another glycerine and remaining pure water are placed in glue pot is heated To 70-80 DEG C, it is well mixed, is subsequently adding the gelatin after expansion, stirring is dissolved, be incubated 1-2h, then stands and cause on foam It is floating, then scrape and defoam, it is filtrated to get glue, heat preservation for standby use with calico;
(2), the glue that will prepare uniformly be applied to flat surface of steel plate, then heating steel sheet so that the water on glue surface Divide evaporation, obtain cushion compound;
B. the preparation of content
Weigh the Tea Pigment powder of preparation in claim 1 and by heat sterilization, the edible vegetable oil clarified in colloid Grinding and fully emulsified, then placement degassing in mill;
C. compacting soft capsule, wash ball, drying, inspection and obtain product.
In the above-mentioned technical solutions:Step A(2)In:The heating-up temperature of steel plate is 90 DEG C.
In the above-mentioned technical solutions:The edible vegetable oil be wheat-germ oil or peanut oil or soybean oil or corn oil or Tea-seed oil or coconut oil or their miscella.
Using above-mentioned technical proposal, obtained Tea Pigment is made soft capsule, it is longer than hard shell capsules, tablet shelf-life, more Instant edible.
Beneficial effect:The present invention has following remarkable advantage:
1. the present invention is with tea fresh leaves as raw material, the Tea Pigment produced, and Main Ingredients and Appearance is high-quality theaflavin and thearubigin, And purity is higher.The present invention can be consumed largely because the unsalable national half area of low and middle-grade tea does not adopt summer tea and autumn tea, in vain wave Take the problem of tea resource.Turn waste into wealth, be that new approach is opened up in summer, the sale of autumn tea, effectively solve the problems, such as the agriculture, rural areas and farmers of tea grower. Tea grower's plantation enthusiasm can be not only improved, also good economic benefit will be brought for Poor Mountainous Area peasant, agricultural industry is developed With induced effect.
2. than water, any organic solvent is not used, without any acid solution and alkali lye, safe, cost yet Extremely low, non-environmental-pollution, also not into the recovery problem in organic solvent, so being saved greatly cost of equipment.
3. continuous countercurrent extraction process equipment used, and raw material carries that most rate is high, recovery rate is high;Tea-water proportion is about legacy equipment 1/3, extraction time is about the 1/6 of legacy equipment, and energy saving is in the range of double figures.
4. nanofiltration concentration is a kind of not covert concentration technique of water, more than vacuum concentration energy-conservation three times(Low-carbon technology), It is to be concentrated into 1.15-1.2/cm in nanofiltration again with vacuum concentration after nanometer concentration3On the basis of be further concentrated to 1.3/cm3 It is a kind of low-carbon energy-saving technology to be spray-dried again, can more conventional spray drying energy-conservation half.
5. the present invention prepare dark brown cellulose soft capsules, be the soft capsule preparation produced as raw material with Tea Pigment, than hard shell capsules, The tablet shelf-life is longer, is more convenient edible.Tea Pigment of the invention can comprehensively act on human body, and its over ride effect is single Lipid-lowering medicine, Thrombolytic Drugs, vasodilator agent, have nine synchronous heavy effects to human body:Bidirectional modulation blood fat, dilute blood viscosity, Anti-freezing, thrombolysis, scavenging activated oxygen(Anti-aging), repair blood vessel endothelium injury, prevention and eliminate microcirculation disorder(Microcirculation The disease that obstacle causes just has kind more than 100;Then obstructed, the no pain by smooth breath of pain), improve blood cell vigor and enhancing human immunity Power.
Specific embodiment
With reference to embodiment, the invention will be further described:
Embodiment 1
The method that Tea Pigment is extracted from tealeaves, completes in accordance with the following steps:
1st, tealeaves pre-treatment:Fresh tea passes are blended into the pastel of 20 mesh or so in meat mincer.Place 4 hours.The fresh tea Leaf may also be and dry or dry or the interior drying of 50oC(Not by de-enzyme)Fresh tea passes.
2nd, above-mentioned pastel is supplied into Continuous Countercurrent Extraction equipment by continuous feeding machine, with 800The hot water of more than C is continuous Adverse current is extracted.
3rd, filter:80 eye mesh screens are crossed, with sharp next step micro-filtration.
4th, micro-filtration:The filtrate of filtering passes through Microfilter(Aperture is 0.5 μm)Carry out micro-filtration.The prefilter of ultrafiltration.
5th, ultrafiltration:Filtrate after micro-filtration is passed through into ultrafilter(Aperture is 100000 dalton)Ultrafiltration is carried out, albumen is filtered The impurity such as matter, pectin, resin, bacterium, starch, it is ensured that the quality of dark brown cellulose soft capsules raw material.
6th, by the filtrate after ultrafiltration through collecting and filtering apparatus(Aperture is 700 dalton)Density is concentrated into for 1.15 g/cm3It is dense Contracting liquid, then density is concentrated in vacuo to for 1.3g/cm3Concentrate.
7th, it is 1.3g/cm by density3Concentrate spray drying, obtain Tea Pigment powder.
8th, crush:To 100 mesh.
9th, packaging and storage:Vacuum sealed package, in order to avoid the moisture absorption.The flavine of obtained product, thearubigin and theabrownin it is total It is 65% to measure, and wherein the content of thearubigin is 22%, and theaflavin content is 13%, and dark brown pigment content is 30%.
Embodiment 2
The method that Tea Pigment is extracted from tealeaves, completes in accordance with the following steps:
1st, tealeaves pre-treatment:Fresh tea passes are blended into the pastel of 40 mesh or so in meat mincer.Place 1 hour.
2nd, above-mentioned pastel is supplied into Continuous Countercurrent Extraction equipment by continuous feeding machine, with 800The hot water of more than C is continuous Adverse current is extracted.
3rd, filter:80 eye mesh screens are crossed, with sharp next step micro-filtration.
4th, micro-filtration:The filtrate of filtering passes through Microfilter(Aperture is 0.5 μm)Carry out micro-filtration.The prefilter of ultrafiltration.
5th, ultrafiltration:Filtrate after micro-filtration is passed through into ultrafilter(Aperture is 100000 dalton)Ultrafiltration is carried out, albumen is filtered The impurity such as matter, pectin, resin, bacterium, starch, it is ensured that the quality of dark brown cellulose soft capsules raw material.
6th, by the filtrate after ultrafiltration through collecting and filtering apparatus(Aperture is 700 dalton)Density is concentrated into for 1.2 g/cm3Concentration Liquid, then density is concentrated in vacuo to for 1.3g/cm3Concentrate.
7th, it is 1.3g/cm by density3Concentrate spray drying, obtain Tea Pigment powder.
8th, crush:To 100 mesh.
9th, packaging and storage:Vacuum sealed package, in order to avoid the moisture absorption.The flavine of obtained product, thearubigin and theabrownin it is total It is 69% to measure, and wherein the content of thearubigin is 24%, and theaflavin content is 14%, and dark brown pigment content is 31%.
Embodiment 3
The preparation of tea pigment capsule:
1st, the preparation of capsule material glue:
1. it is formulated:Gelatin:Glycerine:Pure water:Natural edible carbon black=38:11:49:0.25.
2. step:Taking the gelatin appropriate pure water of addition expands it.Heated during glycerine and remaining pure water separately are put into glue pot To 70-800C, is well mixed, and adds the gelatin stirring of expansion, dissolves, and is incubated 1-2 hour, stands, and foam is floated, and scrapes off The foam of floating, calico filtration, heat preservation for standby use.
2nd, glue piece:The capsule material glue for preparing is taken, is applied on flat surface of steel plate, make thickness uniform, then with 900C The temperature heating of left and right, evaporates surface moisture, as the suitable cushion compound with certain elasticity of toughness.
3rd, the preparation of content:
1. it is formulated:Tea Pigment raw material and corn oil in embodiment 1, the Tea Pigment are 1 with the weight ratio of corn oil: 3。
2. step:Tea Pigment attritive powder is weighed, the corn oil with heated sterilizing, clarification grinds and fill in colloid mill Divide emulsification, place degassing and obtain content emulsion.
4th, soft capsule compacting:Content emulsion is put into hopper, soft capsule is suppressed using rotation die pressing.
5th, ball and drying are washed:Carry out soft capsule and wash ball and drying, the about 0.125g containing Tea Pigment in every.
6th, check:Carry out soft capsule inspection.
7th, packaging and storage:Soft capsule is packed, finished product storage.
Embodiment 4
The preparation of tea pigment capsule:
1st, the preparation of capsule material glue:
1. it is formulated:Gelatin:Glycerine:Pure water:Natural edible annatto pigment=39:12:50:0.3.
2. step:Taking the gelatin appropriate pure water of addition expands it.Heated during glycerine and remaining pure water separately are put into glue pot To 70-800C, is well mixed, and adds the gelatin stirring of expansion, dissolves, and is incubated 1-2 hour, stands, and foam is floated, and scrapes off The foam of floating, calico filtration, heat preservation for standby use.
2nd, glue piece:The capsule material glue for preparing is taken, is applied on flat surface of steel plate, make thickness uniform, then with 900C The temperature heating of left and right, evaporates surface moisture, as the suitable cushion compound with certain elasticity of toughness.
3rd, the preparation of content:
1. it is formulated:The weight of Tea Pigment raw material and wheat-germ oil in embodiment 2, the Tea Pigment and wheat-germ oil Than being 1:4.
2. step:Tea Pigment attritive powder is weighed, the peanut oil with heated sterilizing, clarification is fully newborn in colloid mill Change, place degassing and obtain content emulsion.
4th, soft capsule compacting:Content emulsion is put into hopper, soft capsule is suppressed using rotation die pressing.
5th, ball and drying are washed:Carry out soft capsule and wash ball and drying.
6th, check:Carry out soft capsule inspection.
7th, packaging and storage:Soft capsule is packed, finished product storage.
Embodiment 5
The preparation of tea pigment capsule:
1st, the preparation of capsule material glue:
1. it is formulated:Gelatin:Glycerine:Pure water:Natural edible capsicum red pigment=38.35:11.50:49.87:0.28.
2. step:Taking the gelatin appropriate pure water of addition expands it.Heated during glycerine and remaining pure water separately are put into glue pot To 70-800C, is well mixed, and adds the gelatin stirring of expansion, dissolves, and is incubated 1-2 hour, stands, and foam is floated, and scrapes off The foam of floating, calico filtration, heat preservation for standby use.
2nd, glue piece:The capsule material glue for preparing is taken, is applied on flat surface of steel plate, make thickness uniform, then with 900C The temperature heating of left and right, evaporates surface moisture, as the suitable cushion compound with certain elasticity of toughness.
3rd, the preparation of content:
1. it is formulated:Tea Pigment raw material and soybean oil in embodiment 2, Tea Pigment are 1 with the weight ratio of soybean oil:2.
2. step:Tea Pigment attritive powder is weighed, the wheat-germ oil with heated sterilizing, clarification is abundant in colloid mill Emulsification, places degassing and obtains content emulsion.
4th, soft capsule compacting:Content emulsion is put into hopper, soft capsule is suppressed using rotation die pressing.
5th, ball and drying are washed:Carry out soft capsule and wash ball and drying, the about 0.125g containing Tea Pigment in every.
6th, check:Carry out soft capsule inspection.
7th, packaging and storage:Soft capsule is packed, finished product storage.
Soft capsule prepared by the present invention is carried out into Accelerated stability test:Purchase the soft capsule of present invention preparation and on the market The tablet and hard shell capsules bought are placed six months under conditions of 40 DEG C ± 2 DEG C of temperature, relative humidity 75% ± 5%, during experiment One month, second month, the 3rd month, the 4th month and six month it is separately sampled once, investigate content color and luster, content. It was found that after six months, the color and luster of soft capsule content prepared by the present invention, content are basically unchanged, there is not layering yet Phenomenon.And tablet then had obvious intensification in four month color and luster;Hard capsule content was then occurred as soon as at three month High oxidation becomes dark brown by light brown, and dark brown content is flowed out after a small number of hard shell capsules moisture absorptions.
Soft capsule of the invention was placed up to 5 years at normal temperatures, the color and luster of its content does not also become, and content is basic Stabilization, it is not stratified.This product good stability.
The present invention is not limited to specific embodiment.The raw material middle period of the invention can add some low and middle-grade tealeaves, tea dust, Tea ash does raw material.Edible vegetable oil used by the present invention can also be soybean oil, sesame oil, tea-seed oil, coconut oil etc., not limit to Wheat-germ oil, peanut oil and corn oil in embodiment.As long as it is any equivalent on the basis of of the invention in a word Deformation is each fallen within protection scope of the present invention.The Tea Pigment of present invention production can also cook the food such as tablet, health products and medicine The raw material of product.

Claims (5)

1. a kind of dark brown cellulose soft capsules, are made up of content and capsule material, it is characterised in that:The content is Tea Pigment and eats Vegetable oil, the Tea Pigment is 1 with the weight ratio of edible vegetable oil:2-4;Gained Tea Pigment includes theaflavin, thearubigin and tea Brown element, wherein the total amount of the theaflavin, thearubigin and theabrownin is more than 65%, and the content of thearubigin is more than or equal to 22%, Theaflavin content is more than or equal to 13%, and dark brown pigment content is more than or equal to 30%;
The extracting method of the Tea Pigment is:
(1), will not rub into 20-40 mesh pastel by the tealeaves of de-enzyme treatment, place 1-4h;
(2), with temperature Continuous Countercurrent Extraction is carried out to above-mentioned pastel more than 80 DEG C of hot water;
(3), by extract solution with 80 mesh sieve net filtrations, be then concentrated into extract solution density for 1.15-1.2 through micro-filtration, ultrafiltration, nanofiltration g/cm3, extract solution density is then concentrated in vacuo to again for 1.3g/cm3, then obtain the Tea Pigment by spray drying;
The capsule material is gelatin by according to ratio of weight and number:Glycerine:Pure water:Natural food colour=38-39:11-12:49-50: The raw material of 0.25-0.3 are obtained;
The preparation method of dark brown cellulose soft capsules is:
A, the preparation method of capsule material are:
(a), in gelatin add portion of pure water expand it;Separately glycerine and remaining pure water are placed in glue pot and is heated to 70-80 DEG C, it is well mixed, is subsequently adding the gelatin after expansion, stirring is dissolved, be incubated 1-2h, then stands and cause that foam floats, Scrape again and defoam, glue, heat preservation for standby use are filtrated to get with calico;
(b), the glue that will prepare uniformly be applied to flat surface of steel plate, then heating steel sheet so that the moisture on glue surface steams Hair, obtains cushion compound;
B, the preparation method of content are:
Weigh Tea Pigment powder fully emulsified in colloid mill with by heat sterilization, the edible vegetable oil clarified, then place Degassing obtains content emulsion;
C, soft capsule is suppressed, ball, drying, inspection is washed and is obtained product.
2. dark brown cellulose soft capsules according to claim 1, it is characterised in that:Step(1)In, with stainless steel meat grinder by fresh tea Leaf is rubbed.
3. dark brown cellulose soft capsules according to claim 1, it is characterised in that:Step(3)Material requirement after middle spray drying It is crushed to below 100 mesh.
4. dark brown cellulose soft capsules according to claim 1, it is characterised in that:Step(b)In:The heating-up temperature of steel plate is 90 ℃。
5. dark brown cellulose soft capsules according to claim 1, it is characterised in that:The edible vegetable oil is wheat-germ oil or flower Oil generation or soybean oil or corn oil or tea-seed oil or coconut oil.
CN201410176092.9A 2014-04-29 2014-04-29 Method for extracting tea pigment from tea leaves and tea pigment soft capsule Active CN103908523B (en)

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CN105250261A (en) * 2015-11-19 2016-01-20 成都普瑞法科技开发有限公司 Theaflavin-containing pharmaceutical composition and application thereof in the aspect of lowering blood fat
CN105796493A (en) * 2016-03-31 2016-07-27 中国农业科学院茶叶研究所 Preparation method of theaflavin micro emulsion
CN106213577B (en) * 2016-09-20 2019-01-04 福建中烟工业有限责任公司 Prepare the method and Iron Guanyin water-removing tea extraction of Iron Guanyin water-removing tea extraction
CN106728417A (en) * 2017-01-18 2017-05-31 俞镜含 A kind of gentle method for extracting Tea Pigment
CN111035697A (en) * 2019-12-31 2020-04-21 格律药业有限公司 Pharmaceutical composition and application thereof, preparation method of nanoparticles, extraction process of tea extract and tea extract

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