CN105661519A - Method for preparing healthcare eucommia ulmoides medicine powder through enzymolysis of eucommia ulmoides leaves - Google Patents

Method for preparing healthcare eucommia ulmoides medicine powder through enzymolysis of eucommia ulmoides leaves Download PDF

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Publication number
CN105661519A
CN105661519A CN201610056790.4A CN201610056790A CN105661519A CN 105661519 A CN105661519 A CN 105661519A CN 201610056790 A CN201610056790 A CN 201610056790A CN 105661519 A CN105661519 A CN 105661519A
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enzymolysis solution
eucommia ulmoides
enzymolysis
concentration
protease
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CN201610056790.4A
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张学俊
张萌萌
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Individual
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention discloses a method for preparing healthcare eucommia ulmoides medicine powder through enzymolysis of eucommia ulmoides leaves. The method comprises steps as follows: (1), a eucommia ulmoides leaf basic material is prepared; (2), the stratum corneum on the surface of shred eucommia ulmoides leaves is removed through cutinase; (3), a protein component is removed through protease; (4), pectic substances bonded with the stratum corneum and part of plant cell walls are subjected to enzymolysis through pectinase; (5), the pectic substances bonded with the stratum corneum and part of plant cell walls are continuously subjected to enzymolysis through cellulase, and dissolution of intracellular drug ingredients is facilitated through hydrolysis of the cell walls; (6), the healthcare eucommia ulmoides medicine powder is prepared. According to the method, the stratum corneum on the surface of the eucommia ulmoides leaves is removed firstly through the cutinase, traditional smashing and grinding treatment is replaced, effective ingredients in the eucommia ulmoides leaves are completely protected without damage to an eucommia ulmoides gum structure, eucommia ulmoides gum extraction can be performed on residues while natural substances are extracted, and the method is dual-purpose, efficient and environment-friendly. The method is suitable for processing and utilization of the eucommia ulmoides leaves, eucommia ulmoides bark and eucommia ulmoides peel.

Description

Enzymolysis Folium Eucommiae prepares the method for eucommia health care medicated powder
Technical field
The present invention is relevant with natural drug, also relevant with the process technique of polymer substance, prepares eucommia health care medicated powder in particular to enzymolysis Folium Eucommiae.
Technical background
The Eucommiaceae plant Cortex Eucommiae (Eucommiaulmoides) bark be a kind of rare Chinese medicine, the Cortex Eucommiae is all classified as top grade Chinese medicine by first Chinese Traditional Medicine preciousness books Shennong's Herbal of China, the Compendium of Material Medica of Li Shizhen (1518-1593 A.D.) is also classified as the Cortex Eucommiae as precious Chinese medicine, the Chinese medicine of several thousand facts have proved that the Cortex Eucommiae is tonic herb, returns liver, kidney channel tool invigorating the liver and kidney, bone and muscle strengthening, blood pressure lowering, many effects such as antiabortive. Chinese medicine books are recorded, the Cortex Eucommiae call its " cure mainly waist and knee, invigorating middle warmer, benefit vital essence, hard muscles and bones, wet except itching under the moon, dribbling urination. Clothes for a long time, make light of one's life by commiting suicide resistance to old "; " worry of all parts of the body cavity below the umbilicus, housing the bladder, kidneys and bowels, the non-Cortex Eucommiae is not mended; The part of the body cavity below the umbilicus, housing the bladder, kidneys and bowels is wet, and the non-Cortex Eucommiae is unfavorable; The acid of foot shin, the non-Cortex Eucommiae is not gone; Waist knee joint is pain, and the non-Cortex Eucommiae is not removed ". The research of modern medicine proves that the Cortex Eucommiae truly has several functions and effect: (1) the Cortex Eucommiae is first-chop natural antihypertensive drugs (Harvard University Hu Xiuying professor) in the world; (2) the Cortex Eucommiae is one of four big antiaging agents (Japan professor high bridge week seven) in the world; (3) the Cortex Eucommiae is the excellent fat-reducing drink effectively having no side effect; (4) antifatigue effect; (5) enhancing human body immunity function; (6) calm the nerves, hypnotic; Yang invigorating functions, regulate estrogen; (8) there is removing toxic substances, anti-tumor activity.
In recent years, health problem is day by day concerned. Along with the research that the further investigation of the Cortex Eucommiae and ingredient are extracted, people are while research Gutta extraction, also some health care medicines relevant to the Cortex Eucommiae are developed, for instance Chinese patent application part 200410070200.0 " Qianglitianmaduzhong soft capsule and preparation technology thereof ", No. 201410499693.3 " a kind of Cortex Eucommiae fine powder, eucommia bark polycose and gutta-percha coproduction extraction separation method ", No. 201410601104.8 " a kind of Cortex Eucommiae moxibustion goods and preparation method thereof " etc. But these patented technologies are not yet fully confirmed for the effect of health of people.
Summary of the invention
Research proves, Folium Eucommiae is very much like with the chemical composition of Cortex Eucommiae and pharmacological action, and the exploitation that the characteristic of Cortex Eucommiae deciduous plant is Folium Eucommiae provide solid material base. In the Compendium of Material Medica of Ming Dynasty Li Shizhen (1518-1593 A.D.) work in connection with in the Cortex Eucommiae " nascent tender leaf and spend real can be used as medicinal " record.
It is desirable to provide a kind of method that enzymolysis Folium Eucommiae prepares eucommia health care medicated powder, can effective ingredient in complete extraction Folium Eucommiae, the structure of gutta-percha will not be destroyed again, healthy for people. Service, it is possible to simultaneously produce gutta-percha.
It is with Folium Eucommiae for base material that the enzymolysis Folium Eucommiae that inventor provides prepares the method for eucommia health care medicated powder, through repeatedly enzyme-squash techniqued eucommia health care medicated powder; Concrete grammar includes:
(1) Folium Eucommiae base material is prepared
The Folium Eucommiae wind of screening of learning from else's experience drenches selecting crude drugs with winnower and blows down impurity foreign body, and through rubbing rotten or rolling and fracture and keep former big chip architecture, subpackage is to 3 1000ml triangular flasks or sends in enzymatic vessel;
(2) horny layer of Folium Eucommiae fractal surfaces is removed by
In every triangular flask, add at liquid respectively, and do not rub rotten Eucommia ulmoides Oliv. leaves, and put in shaking bath and react; Collecting enzymolysis solution after reaction, filter with fast grade filter paper, filtering residue is back in triangular flask, collects clear liquid, and samples survey ultraviolet and chromatograph; The concentration that is placed in Rotary Evaporators by the at enzymolysis solution being filtrated to get vacuum, adds dehydrated alcohol to final concentration of 75%~80%. After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
(3) protein component is removed with protease
Weigh protease 4.5g in 500mL beaker, be made into pH buffer with food grade citric acid and sodium citrate, the protease on point 3 lyase preparations, collect the supernatant, after mixing, on average fill in triangular flask; Enzyme digestion reaction, the enzymolysis solution of collection 3 bottles after reaction, merging enzymolysis solution, the filtration on shaking table when optimum pH, ultraviolet and chromatograph are surveyed in sampling, and filtering residue is back in triangular flask; Then the concentration that is placed in Rotary Evaporators by enzymolysis solution filtrate vacuum, adds dehydrated alcohol to final concentration of 75%~80%. After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
(4) pectic substance and the Activities of Some Plants cell wall of interconnection function between pectinase enzymatic hydrolysis and horny layer and cell wall are used
Afterwards, weighing pectase in 500mL beaker, regulating pH with food stage citric acid and sodium citrate is 4.5, and the pectase on point 3 lyase preparations is collected the supernatant, after mixing, on average filled in triangular flask; Enzyme digestion reaction, the enzymolysis solution of collection 3 bottles after reaction, merging enzymolysis solution, the filtration on shaking table when optimum pH, ultraviolet and chromatograph are surveyed in sampling, and filtering residue is back in triangular flask; Then the concentration that is placed in Rotary Evaporators by enzymolysis solution filtrate vacuum, adds dehydrated alcohol to final concentration of 75%~80%; After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
(5) continue the cell wall of enzymolysis of plants cell tissue with cellulase, the hydrolysis of cell wall is conducive to the dissolution of ingredient in born of the same parents
Weigh citric acid and sodium citrate, be dissolved in 1500mL water, to pH ≈ 5.0, standby; Extracting cellulose enzyme, in 500mL beaker, divides the cellulase protein on three lyase preparations with standby citric acid-sodium solution, collects the supernatant, after mixing, on average fills in triangular flask;Enzyme digestion reaction, the enzymolysis solution of collection 3 bottles after reaction, merging enzymolysis solution, the filtration on shaking table when optimum pH, ultraviolet and chromatograph are surveyed in sampling; Then the concentration that is placed in Rotary Evaporators by enzymolysis solution filtrate vacuum, adds dehydrated alcohol to final concentration of 75%~80%; After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
(6) the preparation of eucommia health care medicated powder
Weigh 50g beta-schardinger dextrin-in rotary evaporation bottle, to add in the evaporative flask filling beta-schardinger dextrin-by amount through the at enzymolysis solution of Ethanol Treatment, protease hydrolyzed liquid, pectinase enzymatic hydrolysis liquid, the cellulase degradation liquid supernatant, it is evaporated on a rotary evaporator, size-reduced machine is pulverized, final prepared eucommia health care medicated powder.
In the of said method (1) step, the every bottled Folium Eucommiae fragment 50~100g of described triangular flask.
In the of said method (2) step, the at liquid measure of described interpolation is 500ml; In described shaking bath, the temperature of reaction is 40 DEG C, response time 24h; The amount of described collection enzymolysis solution is every bottle of 500ml; Amount after the concentration of described vacuum is 100ml.
In the of said method (3) step, described optimum pH condition is pH ≈ 4.0; The temperature of described enzyme digestion reaction is 45 DEG C, response time 24h; The concentration of described vacuum to 100ml.
In the of said method (4) step, the amount of described pectase is 4.5g, accounts for material 3%; The temperature of described enzyme digestion reaction is 50 DEG C, response time 16~24h; Amount after the concentration of described vacuum is 100ml.
In the of said method (5) step, the amount of described cellulase is 4.5g, accounts for material 3%; Described optimum pH condition is pH ≈ 5.0; The temperature of described enzyme digestion reaction is 50 DEG C, response time 16h; Amount after the concentration of described vacuum is 100ml.
In the of said method (6) step, described enzymolysis solution is 500ml; It is 45 DEG C that the temperature being evaporated on described Rotary Evaporators controls, and rotating speed controls as 4r/min.
The inventive method prepare eucommia health care medicated powder usage be oral, every day 2 minor tick 8h, each 3g, warm boiled water.
Inventors have noted that, the inventive method is possible not only to enzymolysis Folium Eucommiae, the inventive method all can be adopted to carry out enzymolysis eucommia bark, Cortex Eucommiae peel, prepares eucommia health care medicated powder.
Satisfied health-care effect is obtained after multidigit old docter of TCM and middle-aged and elderly people take. The old docter of TCM of 4 one's mid-60s each serve on 7 days, all feels: soreness of the waist and knees disappears, hale and hearty, sleeps fabulous, and blood pressure stabilization does not fluctuate. Wherein having 1 people to forget daytime to eat, remember at 11 in evening and eat, the result spirit very night is pure and has a sleepless night, and second day spirit does not still have tired sensation very well; And the people's sleep very well in evening normally taken, urine is reduced. 4 people unanimously think Cortex Eucommiae fine powder health-care effect clearly. Other taken people of Cortex Eucommiae fine powder all constantly persistently incoming call ask for Cortex Eucommiae fine powder and continue to take, the effect that they realize vividly and regulate body function, improve immunocompetence: no longer shed tears after having the taking of phenomenon of shedding tears, and gradually feel in vigorous health many, physical ability strengthens; After the women having hypertension takes, blood pressure is normally steady, and the also recovery originally having menoxenia is normal; After beauty parlor of Korea S uses, feedback says there is obvious cosmetic result for women.
Present invention at first removes the horny layer on Folium Eucommiae surface; instead of traditional pulverizing and roll process; be conducive to the effective ingredient in complete protection Folium Eucommiae; and the structure of gutta-percha will not be destroyed; while extracting natural materials, residue can also be carried out the extraction of gutta-percha; kill two birds with one stone, high-efficiency environment friendly.Processing and utilization suitable in Folium Eucommiae, eucommia bark and Cortex Eucommiae peel.
Detailed description of the invention
Embodiment
The Folium Eucommiae cleaning water of screening of learning from else's experience cleans up, through rubbing rotten or rolling to fracture and fragmentate, subpackage to 3 1000ml triangular flasks, every bottled Folium Eucommiae fragment 100g.
Then, in every triangular flask, add at liquid 500ml respectively, do not have Folium Eucommiae fragment, put and shaking bath reacts at 40 DEG C 24h; Collect enzymolysis solution after reaction, filter with fast grade filter paper, collect clear liquid 500ml, and sample survey ultraviolet and chromatograph for every bottle; It is placed in Rotary Evaporators by the at enzymolysis solution being filtrated to get vacuum and is concentrated into 100ml, add dehydrated alcohol to final concentration of 75%~80%. After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
Then, weigh protease 4.5g in 500mL beaker, be made into pH ≈ 4.0 buffer with food grade citric acid and sodium citrate, the protease on point 3 lyase preparations, collect the supernatant, after mixing, on average fill in triangular flask; Enzyme digestion reaction 24h, each 500ml of enzymolysis solution of collection 3 bottles after reaction, merging enzymolysis solution, filtration at 40 DEG C on shaking table under pH ≈ 4.0 condition, ultraviolet and chromatograph are surveyed in sampling; Then it is placed in Rotary Evaporators by enzymolysis solution filtrate vacuum and is concentrated into 100ml, add dehydrated alcohol to final concentration of 75%~80%. After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
Afterwards, weighing the pectase 4.5g accounting for material 3% in 500mL beaker, regulating pH with food stage citric acid and sodium citrate is 4.5, and the pectase on point 3 lyase preparations is collected the supernatant, after mixing, on average filled in triangular flask; Enzyme digestion reaction 24h at 50 DEG C on shaking table, collects each 500ml of enzymolysis solution of 3 bottles, merges enzymolysis solution, filter after reaction, ultraviolet and chromatograph are surveyed in sampling; Then it is placed in Rotary Evaporators by enzymolysis solution filtrate vacuum and is concentrated into 100ml, add dehydrated alcohol to final concentration of 75%~80%; After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
Then, weigh the cellulase accounting for material 3%, citric acid and sodium citrate 4.5g and be dissolved in 1500mL water, to pH ≈ 5.0, standby; Extracting cellulose enzyme, in 500mL beaker, divides the cellulase protein on three lyase preparations with standby citric acid-sodium solution, collects the supernatant, after mixing, on average fills in triangular flask; Enzyme digestion reaction 16h, each 500ml of enzymolysis solution of collection 3 bottles after reaction, merging enzymolysis solution, filtration at 50 DEG C on shaking table under pH ≈ 5.0 condition, ultraviolet and chromatograph are surveyed in sampling; Then it is placed in Rotary Evaporators by enzymolysis solution filtrate vacuum and is concentrated into 100ml, add dehydrated alcohol to final concentration of 75%~80%; After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
Finally, weigh 50g beta-schardinger dextrin-in rotary evaporation bottle, by through the at enzymolysis solution of Ethanol Treatment, protease hydrolyzed liquid, pectinase enzymatic hydrolysis liquid, each 500ml of cellulase degradation liquid the supernatant by amount add to contain beta-schardinger dextrin-evaporative flask in, it is evaporated on a rotary evaporator, it is evaporated temperature and controls 45 DEG C, rotating speed controls 4r/min, and size-reduced machine is pulverized, final prepared eucommia health care medicated powder.

Claims (7)

1. the method that enzymolysis Folium Eucommiae prepares eucommia health care medicated powder, it is characterised in that including:
(1) Folium Eucommiae base material is prepared
The Folium Eucommiae wind of screening of learning from else's experience drenches selecting crude drugs with winnower and blows down impurity foreign body, and through rubbing rotten or rolling and fracture and keep former big chip architecture, subpackage is to 3 1000ml triangular flasks or sends in enzymatic vessel;
(2) horny layer of Folium Eucommiae fractal surfaces is removed by
In every triangular flask, add at liquid respectively, do not have Folium Eucommiae fragment, and put in shaking bath and react; Collect enzymolysis solution after reaction, filter with fast grade filter paper, collect clear liquid, and sample survey ultraviolet and chromatograph; The concentration that is placed in Rotary Evaporators by the at enzymolysis solution being filtrated to get vacuum, adds dehydrated alcohol to final concentration of 75%~80%; After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
(3) remove protein component with protease (can be selected for acid protease, neutral protease, alkaline protease) and destroy fabric structure
Weigh protease 4.5g in 500mL beaker, be made into pH buffer with food grade citric acid and sodium citrate, the protease on point 3 lyase preparations, collect the supernatant, after mixing, on average fill in triangular flask; Enzyme digestion reaction, the enzymolysis solution of collection 3 bottles after reaction, merging enzymolysis solution, the filtration on shaking table when optimum pH, ultraviolet and chromatograph are surveyed in sampling; Then the concentration that is placed in Rotary Evaporators by enzymolysis solution filtrate vacuum, adds dehydrated alcohol to final concentration of 75%~80%; After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
(4) pectic substance being adhered with pectinase enzymatic hydrolysis and horny layer and Activities of Some Plants cell wall
Afterwards, weighing pectase in 500mL beaker, regulating pH with food stage citric acid and sodium citrate is 4.5, and the pectase on point 3 lyase preparations is collected the supernatant, after mixing, on average filled in triangular flask; Enzyme digestion reaction, the enzymolysis solution of collection 3 bottles after reaction, merging enzymolysis solution, the filtration on shaking table when optimum pH, ultraviolet and chromatograph are surveyed in sampling; Then the concentration that is placed in Rotary Evaporators by enzymolysis solution filtrate vacuum, adds dehydrated alcohol to final concentration of 75%~80%; After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
(5) continue the cell wall of enzymolysis of plants cell tissue with cellulase, the hydrolysis of cell wall is conducive to the dissolution of ingredient in born of the same parents
Weigh citric acid and sodium citrate, be dissolved in 1500mL water, to pH ≈ 5.0, standby; Extracting cellulose enzyme, in 500mL beaker, divides the cellulase protein on three lyase preparations with standby citric acid-sodium solution, collects the supernatant, after mixing, on average fills in triangular flask; Enzyme digestion reaction, the enzymolysis solution of collection 3 bottles after reaction, merging enzymolysis solution, the filtration on shaking table when optimum pH, ultraviolet and chromatograph are surveyed in sampling; Then the concentration that is placed in Rotary Evaporators by enzymolysis solution filtrate vacuum, adds dehydrated alcohol to final concentration of 75%~80%; After adding ethanol, enzymolysis solution there will be partly precipitated, takes supernatant and is loaded on cyclodextrin, and precipitation is collected separately;
(6) the preparation of eucommia health care medicated powder
Weighing 50g beta-schardinger dextrin-in rotary evaporation bottle, add in the evaporative flask filling beta-schardinger dextrin-by the enzymolysis solution supernatant of the various enzymes through Ethanol Treatment by amount, be evaporated on a rotary evaporator, size-reduced machine is pulverized, final prepared eucommia health care medicated powder;
Process with this same procedure through the at enzymolysis solution of Ethanol Treatment, protease hydrolyzed liquid, pectinase enzymatic hydrolysis liquid, cellulase degradation liquid, prepare eucommia health care medicated powder.
2. in accordance with the method for claim 1, it is characterised in that the (1) in step, the every bottled Folium Eucommiae fragment 50~100g of described triangular flask.
3. in accordance with the method for claim 1, it is characterised in that the (2) in step, and the at liquid measure of described interpolation is 500ml; In described shaking bath, the temperature of reaction is 40 DEG C, response time 24h; The amount of described collection enzymolysis solution is every bottle of 500ml; Amount after the concentration of described vacuum is 100ml.
4. in accordance with the method for claim 1, it is characterised in that the (3) in step, and described optimum pH condition is pH ≈ 4.0; The temperature of described enzyme digestion reaction is 45 DEG C, response time 24h; The concentration of described vacuum to 100ml.
5. in accordance with the method for claim 1, it is characterised in that the (4) in step, and the amount of described pectase is 4.5g, accounts for material 3%; The temperature of described enzyme digestion reaction is 50 DEG C, response time 16~24h; Amount after the concentration of described vacuum is 100ml.
6. in accordance with the method for claim 1, it is characterised in that the (5) in step, and the amount of described cellulase is 4.5g, accounts for material 3%; Described optimum pH condition is pH ≈ 5.0; The temperature of described enzyme digestion reaction is 50 DEG C, response time 16h; Amount after the concentration of described vacuum is 100ml.
7. in accordance with the method for claim 1, it is characterised in that the (6) in step, and described enzymolysis solution is each 500ml; It is 45 DEG C that the temperature being evaporated on described Rotary Evaporators controls, and rotating speed controls as 4r/min.
CN201610056790.4A 2016-01-28 2016-01-28 Method for preparing healthcare eucommia ulmoides medicine powder through enzymolysis of eucommia ulmoides leaves Pending CN105661519A (en)

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CN106912677A (en) * 2017-01-19 2017-07-04 浙江旭源杜仲生物科技有限公司 Nonreactive eucommia feed
CN106954852A (en) * 2017-01-19 2017-07-18 浙江旭源杜仲生物科技有限公司 Health care bark of eucommia fine powder
CN107637744A (en) * 2017-09-29 2018-01-30 贵州五新农业科技有限责任公司 Bark of eucommia solid beverage and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106912677A (en) * 2017-01-19 2017-07-04 浙江旭源杜仲生物科技有限公司 Nonreactive eucommia feed
CN106954852A (en) * 2017-01-19 2017-07-18 浙江旭源杜仲生物科技有限公司 Health care bark of eucommia fine powder
CN107637744A (en) * 2017-09-29 2018-01-30 贵州五新农业科技有限责任公司 Bark of eucommia solid beverage and preparation method thereof

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Application publication date: 20160615