CN1386744A - Process for extracting triterpenic acid from gleditschia, and medical use and Chinese medicine of triterpenic acid - Google Patents

Process for extracting triterpenic acid from gleditschia, and medical use and Chinese medicine of triterpenic acid Download PDF

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Publication number
CN1386744A
CN1386744A CN 02109825 CN02109825A CN1386744A CN 1386744 A CN1386744 A CN 1386744A CN 02109825 CN02109825 CN 02109825 CN 02109825 A CN02109825 A CN 02109825A CN 1386744 A CN1386744 A CN 1386744A
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honey locust
acid
chinese honey
triterpenic acid
ethanol
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CN1169825C (en
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赵全成
王本祥
陈声武
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Sichuan Jishengtang Pharmaceutical Co ltd
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TIANYAO SCIENCE AND TECHNOLOGY Co Ltd JILIN
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Abstract

A process for extracting triterpenic acid from gleditschia includes extracting in alcohol, decolouring, fitlering, recovering alcohol, diluting with deionized water, purifying by macroporous adsorption resin column, eluting, concentrating, drying to obtain triterpene saponin, adding it to 2N sulfuric acid or alcohol solution, degradating insoluble substance, washing with water to remove excessive acid, dissolving, decolouring, filtering, crystallizing and drying. Said extract can be used to prepare medicine for treating and preventing hyperlipomia, fatty liver and atheroma.

Description

From Chinese honey locust, extract the method for triterpenic acid and the medicinal use and the Chinese medicine preparation of triterpenic acid
Technical field:
The present invention discloses a kind of method of triterpenic acid and the medicinal use and Chinese medicine preparation of triterpenic acid of extracting, the extraction preparation method and its usage technical field of pharmaceutically active ingredient in belonging to from Chinese honey locust.
Background technology:
Chinese honey locust (Gleditsia Sinesis Lam.) as Chinese medicine, has sensible, phlegm-dispelling functions, cures mainly apoplexy, mouth is kept silent and disease such as asthma due to excessive phlegm.Chinese honey locust contains abundant triterpenoid saponin, and mucous membrane is had pungency, and phlegm-dispelling functions is arranged, in the traditional Chinese medical science Chinese honey locust treatment commonly used the air port keep silent, stupor etc., belong to the class Chinese medicine of having one's ideas straightened out.Be that raw material extracts in a large number and prepares triterpenic acid and be used for hyperlipidemia disease and suppress cholesterol absorption and do not appear in the newspapers so far with the Chinese honey locust.
Summary of the invention:
The invention discloses a kind of method of extracting the Chinese honey locust triterpenic acid from Chinese honey locust, purpose is intended to extract the Chinese honey locust triterpenic acid with pharmaceutical use from Chinese honey locust, is applicable to suitability for industrialized production.
Another object of the present invention provides the medicine that the Chinese honey locust triterpenic acid is made, and is used for the prevention and the treatment of hyperlipidaemia, suppresses the absorption of cholesterol simultaneously.
Further purpose of the present invention provides the purposes of said extracted thing aspect the medicine of preparation treatment malignant tumour.
Technical solution of the present invention may further comprise the steps:
1, the extraction of total triterpenoid saponin: get the Chinese medicine spaonin powder and be broken into 50~70% the extraction using alcohol three times that fine powder about 20 orders adds 5~9 times, or,, filter with the decolouring of 2% medical active carbon with the decoction alcohol precipitation method extraction, reclaim ethanol, with the deionized water dilution,, use earlier deionized water again through the macroporous adsorptive resins purifying, use 50~70% ethanol elutions again, decompression recycling ethanol, the concentrated solution drying gets total triterpene saponins.
2, the middle degraded of sulfuric acid, ethanolic soln (alcohol concn is 45%) that total triterpene saponins is added hydrochloric acid or the 2N of 2N, the unnecessary acid of filtrate insolubles water flush away, use 85% dissolve with ethanol again, add 3% decolorizing with activated carbon, filter, reclaim ethanol to 1/2 of original volume, place, crystallization filters, drying promptly gets the Chinese honey locust triterpenic acid.
The water that preferably contains 60%~85% ethanol and 40%~15% in preparation technology's extraction using alcohol process of the present invention.
The water that preferably preferably contains 70% ethanol and 30% in the Chinese honey locust triterpenic acid preparation technology extraction using alcohol process of the present invention.
Preferred used hydrochloric acid and sulfuric acid concentration in Chinese honey locust triterpenic acid preparation technology part hydrochloric acid of the present invention or the sulfuric acid degradation process.
Chinese honey locust triterpenic acid of the present invention prepares in the part degradation process, preferably contains 1~3N hydrochloric acid or 1~3N vitriolic, 30%~50% ethanolic soln, degrades 2~5 hours for 100 ℃.
Chinese honey locust triterpenic acid of the present invention prepares in the part degradation process, and best optimum condition is to contain 2N hydrochloric acid or 2N vitriolic 45 ethanolic solns, degrades 3 hours for 100 ℃.
Medicine of the present invention preferably contains 1%~99% Chinese honey locust triterpenic acid and 99%~1% vehicle.
Medicine of the present invention preferably contains 10%~90% Chinese honey locust triterpenic acid and 90%~10% pharmaceutical excipient.
Medicine of the present invention preferably contains 30%~80% Chinese honey locust triterpenic acid and 70%~20% pharmaceutical excipient.
Medicine of the present invention preferably contains 60%~70% Chinese honey locust triterpenic acid and 40%~30% vehicle.
It is activeconstituents that medicine of the present invention contains the extract for the treatment of significant quantity, and contains one or more pharmaceutically acceptable carriers.
Extract of the present invention can be used for preparing the medicine of treatment and diseases such as prevention hyperlipidemia, fatty liver and atheroma.
The present invention can composition form be applied to the patient of this treatment by oral, rectum, vein, intramuscular injection or parenteral admin mode.Prepare various formulations as tablet, granule, electuary, capsule, suppository, sprays, sustained release dosage, liquid oral formulation and injection according to the conventional production method of pharmaceutical field.Also can make its activeconstituents and one or more carriers or medicament mixed, make required formulation.
Carrier above is meant the pharmaceutical carrier of pharmaceutical field routine, comprises as sanitas, pigment, thinner, vehicle, weighting agent, tackiness agent, correctives, wetting agent, disintegrating agent, absorption enhancer, tensio-active agent, absorption carrier.
Pharmaceutical composition preferred weight ratio of the present invention is 0.1%~99.5% activeconstituents.
Formulation rate of the present invention can be according to variations such as route of administration, patient age, body weight, disease type and severity, and per daily dose is 0.01~10mg/kg.
The drug effect of Chinese honey locust triterpenic acid:
Chinese honey locust triterpenic acid chmice acute toxicity test shows that when the gastric infusion maximum tolerated dose was 20g/kg, animal did not have death, and Chinese honey locust triterpenic acid non-toxic reaction is described.The Chinese honey locust triterpenic acid has the effect of lipidemia disease and suppresses the effect of cholesterol absorption, is verified by following experiment.
1, the Chinese honey locust triterpenic acid is to the prophylactic action of experimental rat hyperlipidaemia
Materials and methods
70 of animal male wistar rats, body weight 200~250g is available from the high-new Experimental Animal Center in Changchun.
Medicine Chinese honey locust triterpenic acid white powder is provided by this institute plant chamber; DIAOXINXUE KANG JIAONANG, specification: 100mg/ grain, lot number 0201044, Chengdu Diao Pharmaceutical Group Co., Ltd of Chinese Academy of Sciences product; Nicotinic acid tablet, specification: the 100mg/ sheet, lot number: 990801, Shanghai nine good fortune Pharma Inc. products; Cholesterol, specification: analytical pure, the 500g/ bottle, lot number: 993538, the emerging chemical reagent in Shanghai institute product; Propylthiouracil, specification: the 50mg/ sheet, lot number: 010806, Shanghai Fosun Zhaohui Pharmaceutical Co., Ltd. (morning sunlight pharmaceutical factory of former The 2nd Army Medical College) product.Total cholesterol (TC) detection kit, lot number: 020101, give birth to biotechnology engineering hi-tech department product in Beijing.
Instrument TU-1800S type ultraviolet-visible pectrophotometer, Beijing Puxi General Instrument Co., Ltd's product.
After the method laboratory animal was bought, routine feeding also conformed for 1 week it, was divided into normal control, hyperlipidemia model, nicotinic acid tablet (300mg.kg then at random -1), Diaoxinxuekang (400mg.kg -1), Chinese honey locust triterpenic acid (200,100 and 50mg.kg -1) totally 7 groups.Every group 10.The first stomach of irritating of every morning every animal gives high lipoprotein solution 10mlkg -1(wherein, lard 10g+ cholesterol 2g+ propylthiouracil 0.2g is dissolved in 0.5% Xylo-Mucine), (volume is 5mlkg to gavage different pharmaceutical according to grouping subsequently -1).The normal control treated animal is irritated stomach and is given equal-volume distilled water.Successive administration 14d.After 12 hours, with 10% Chloral Hydrate (4ml/kg) ip anesthesia, through abdominal aortic blood, separation of serum is measured serum total cholesterol content with animal in last administration (water is can't help in fasting).
The result
Chinese honey locust triterpenic acid preventive administration sees Table 1 to the influence of hyperlipidemia rats serum total cholesterol content.Table 1. Chinese honey locust triterpenic acid capsule is to the influence of experimental hyperlipidemia rat blood serum total cholesterol level (x ± s)
The grouping of dosage number of animals serum TC content
(mg/kg) (only) (mmol/L) normal control---10 2.22 ± 0.65 * *Hyperlipidemia model---10 5.79 ± 1.30 nicotinic acid tablets 300 10 3.89 ± 0.87 *Diaoxinxuekang 400 10 3.97 ± 0.77 *Chinese honey locust triterpenic acid 200 10 4.19 ± 1.18 *Chinese honey locust triterpenic acid 100 10 4.68 ± 2.03 #Chinese honey locust triterpenic acid 50 10 5.06 ± 1.00 #
Annotate: compare with the hyperlipidemia model group *P<0.05, *P<0.01, * *P<0.001, #P>0.05
The result shows that the Chinese honey locust triterpenic acid can obviously improve the caused hypercholesterolemia lipidemia of rats gavaged cholesterol.
2, the Chinese honey locust triterpenic acid is to the prophylactic action of experimental mouse hyperlipidemia
Used material, instrument, raw material and the animal-origin of this experiment tested 1 rat test part together.(60 of Kunming mouses of method experiment, male and female half and half), after buying, feed routinely and it is conformed a week, be divided into 6 groups at random, be respectively high, medium and low three the dosage groups of blank group, model control group, nicotinic acid control group and Chinese honey locust triterpenic acid, except that the blank group gives normal feed, all the other 5 groups all give high lipid food, when giving feed, blank group and model group are irritated stomach distilled water (0.2mL/10g) every day, irritate stomach nicotinic acid (aqueous solution) and three dosage of Chinese honey locust triterpenic acid (0.5%CMC suspension) respectively for remaining four groups.The altogether administration 15 days of each group, in fasting in night in the 14th day, after the administration in the 15th day 1 hour, eye socket was got blood, 37 ℃ of incubations 30 minutes, centrifugal, 10000r.p.m gets serum 200 μ L, add distilled water 200 μ L, mixing, last automatic biochemical analyzer is measured, and the result is as follows.
(n=10 group dosage (mg/kg) serum cholesterol (mmoL/L) of X ± S) is blank distilled water po 3.08 ± 0.782. model contrast distilled water po 11.83 ± 3.11 1. to the influence of cholesterol in the mice serum for table 2. Chinese honey locust triterpenic acid * *3. nicotinic acid 600po 6.57 ± 1.90 *4. Chinese honey locust triterpenic acid high dosage 2000po 4.78 ± 1.20 *5. dosage 1000po 5.96 ± 2.50 in the Chinese honey locust triterpenic acid *6. Chinese honey locust triterpenic acid low dosage 500po 7.14 ± 2.70 *
Annotate: compare * P<0.05, * * P<0.01, * * * p<0.001 with negative control group
For further confirming the decreasing cholesterol effect of Chinese honey locust triterpenic acid, therefore change dosage, repeat this experiment.
(n=10 group dosage (mg/kg) serum cholesterol (mmoL/L) of X ± S) is blank distilled water po 1.12 ± 0.272. model contrast distilled water po 4.64 ± 3.79 1. to the influence of cholesterol in the mice serum for table 3. Chinese honey locust triterpenic acid * *3. nicotinic acid 600 po 2.31 ± 0.83 *4 Chinese honey locust triterpenic acid high dosages, 500 po 1.95 ± 0.61 *Dosage 250 po 2.46 ± 0.81 in the 5 Chinese honey locust triterpenic acids *6. Chinese honey locust triterpenic acid low dosage 125 po 2.61 ± 1.05 *
The result shows that the Chinese honey locust triterpenic acid can obviously improve the caused hyperlipidemia of mouse gavaging cholesterol.
The Chinese honey locust triterpenic acid is to the influence of experimental hyperlipidemia hemorheology of rat
70 of animal male wistar rats, body weight 200~250g is available from the high-new Experimental Animal Center in Changchun.
Medicine Chinese honey locust triterpenic acid white powder is provided by this institute plant chamber; DIAOXINXUE KANG JIAONANG, specification: 100mg/ grain, lot number 0201044, Chengdu Diao Pharmaceutical Group Co., Ltd of Chinese Academy of Sciences product; Nicotinic acid tablet, specification: the 100mg/ sheet, lot number: 990801, Shanghai nine good fortune Pharma Inc. products; Cholesterol, specification: analytical pure, the 500g/ bottle, lot number: 993538, the emerging chemical reagent in Shanghai institute product; Propylthiouracil, specification: the 50mg/ sheet, lot number: 010806, Shanghai Fosun Zhaohui Pharmaceutical Co., Ltd. (morning sunlight pharmaceutical factory of former The 2nd Army Medical College) product; Total cholesterol (TC) detection kit, lot number: 020101, give birth to biotechnology engineering High-tech company product in Beijing.
Instrument Beijing Puli gives birth to LBY-N6A type self-stip rotational viscosimeter.
After the method laboratory animal was bought, routine feeding also conformed for 1 week it, was divided into normal control, hyperlipidemia model, nicotinic acid tablet (300mg.kg then at random -1), Diaoxinxuekang (400mg.kg -1), Chinese honey locust triterpenic acid (200,100 and 50mg.kg -1) totally 7 groups.Every group 10.The first stomach of irritating of every morning every animal gives high lipoprotein solution 10mlkg -1(wherein, lard 10g+ cholesterol 2g+ propylthiouracil 0.2g is dissolved in 0.5% Xylo-Mucine), (volume is 5mlkg to gavage different pharmaceutical according to grouping subsequently -1).The normal control treated animal is irritated stomach and is given equal-volume distilled water.Successive administration 14d., animal is anaesthetized with 10% Chloral Hydrate (4ml/kg) ip, after 12 hours in last administration (water is can't help in fasting) through abdominal aortic blood 3.5mL, anticoagulant heparin.Give birth to LBY-N6A type self-stip rotational viscosimeter with Beijing Puli and measure hemorheological property.
The result
Hemorheological influence sees Table 4 to Chinese honey locust triterpenic acid preventive administration to hyperlipidemia rats.
Table 4. Chinese honey locust triterpenic acid is to the influence of experimental hyperlipidemia hemorheology of rat (x ± s)
Dosage example whole blood viscosity whole blood viscosity whole blood viscosity plasma viscosity grouping (mg/kg) number is low to be cut/cut in 10/40 height cut/120 120 (1/S)
(only) be (1/S) (1/S) normal control (1/S)---and 10 13.9 ± 2.0 * *7.82 ± 1.01 * *5.56 ± 0.60 * *1.61 ± 0.27 *Hyperlipidemia model---10 25.6 ± 3.6 12.4 ± 1.11 8.20 ± 0.55 2.19 ± 0.39 nicotinic acid tablets 300 10 14.5 ± 1.1 * *7.86 ± 0.59 * *5.60 ± 0.57 * *1.57 ± 0.05 * *Diaoxinxuekang 400 10 17.4 ± 2.9 * *9.66 ± 1.40 * *6.66 ± 0.84 * *1.52 ± 0.08 * *Chinese honey locust triterpenic acid 200 10 17.5 ± 2.7 * *10.1 ± 1.50 *7.25 ± 0.86 *2.12 ± 0.42 #Chinese honey locust triterpenic acid 100 10 16.4 ± 2.3 * *9.16 ± 1.24 * *6.24 ± 0.82 * *2.05 ± 0.41 #Chinese honey locust triterpenic acid 50 10 17.9 ± 1.7 * *10.0 ± 0.66 * *7.07 ± 0.37 * *1.95 ± 0.14 #
Annotate: compare with the hyperlipidemia model group *P<0.05, *P<0.01, * *P<0.001, #P>0.05.
The result shows that the Chinese honey locust triterpenic acid can obviously improve the hemorheological properties of experimental hyperlipidemia rat.Whole blood viscosity of administration animal (low cut, in cut and height is cut) and plasma viscosity all obviously fall in model group.
Embodiment:
Embodiment 1
1 kilogram of Chinese medicine Chinese honey locust, extraction using alcohol with 70% three times, for the first time with 4000 milliliters of 70% ethanol, refluxing extraction 3 hours for the second time with 3000 milliliters of refluxing extraction of 70% ethanol 2 hours, is used 3000 milliliters of refluxing extraction of 70% ethanol 1.5 hours for the third time, merge No. three times extracting solution, with the decolouring of 2% medical active carbon, filter, reclaim ethanol, be diluted to 1500 milliliters with deionized water again, (6cm * 100cm) go up purifying with 3000 milliliters of deionized waters, uses 4000 milliliters of wash-outs of 70% ethanol earlier again at the D101 macroporous adsorbent resin, collect 70% ethanol eluate, decompression recycling ethanol, the concentrated solution drying gets total triterpene saponins.
Get 1 kilogram of total triterpene saponins, add 10000 milliliters and contain the hydrochloric acid of 2N or the ethanol solution of sulfuric acid of 2N (alcohol concn is 45%), degraded is 3 hours under 100 ℃ of conditions, the unnecessary acid of filtrate insolubles water flush away, use 85% dissolve with ethanol again, add 3% decolorizing with activated carbon, filter, reclaim ethanol to 1/2 of original volume, place, crystallization filters, drying promptly gets the Chinese honey locust triterpenic acid.
Practical example 1:
Chinese honey locust triterpenic acid 1kg, medical starch 1kg, 50% ethanol is an amount of, granulates, whole grain, oven dry, dress 1# capsule, every 0.2g.
Other project should meet 2000 editions tablet projects of Pharmacopoeia of People's Republic of China relevant requirements.
Practical example 2:
Chinese honey locust triterpenic acid 1kg, starch 0.6kg, dextrin 0.1kg, 50% ethanol is an amount of, granulates, whole grain, oven dry, compressing tablet, every 0.3g.
Other project should meet 2000 editions capsule projects of Pharmacopoeia of People's Republic of China relevant requirements.
Practical example 3
Take by weighing Chinese honey locust triterpenic acid 100g (95% purity), sodium-chlor usual amounts, 1.1-propylene glycol 50g, adding distil water is an amount of, sodium hydroxide solution with 1~5% is transferred PH8.0, adding distil water 10000ml, after filtration, can and sterilization under aseptic condition, make 5000 of Chinese honey locust triterpenic acid injections, every contains Chinese honey locust triterpenic acid 20mg.

Claims (12)

1, a kind of method of extracting the Chinese honey locust triterpenic acid from Chinese honey locust comprises following processing step:
1) extraction of total triterpenoid saponin: get the Chinese medicine spaonin powder and be broken into 50~70% the extraction using alcohol three times that fine powder about 20 orders adds 5~9 times, or,, filter with the decolouring of 2% medical active carbon with the decoction alcohol precipitation method extraction, reclaim ethanol, with the deionized water dilution,, use earlier deionized water again through the macroporous adsorptive resins purifying, use 50~70% ethanol elutions again, decompression recycling ethanol, the concentrated solution drying gets total triterpene saponins;
2) total triterpene saponins is added degraded in the sulfuric acid, ethanolic soln (alcohol concn is 45%) of the hydrochloric acid of 2N or 2N, the unnecessary acid of filtrate insolubles water flush away, use 85% dissolve with ethanol again, add 3% decolorizing with activated carbon, filter, reclaim ethanol to 1/2 of original volume, place, crystallization filters, drying promptly gets the Chinese honey locust triterpenic acid.
2, method according to claim 1 is characterized in that: the water that preferably contains 60%~85% ethanol and 40%~15% in the extraction using alcohol process.
3, method according to claim 1 is characterized in that: the best water that contains 70% ethanol and 30% in the extraction using alcohol process.
4, method according to claim 1 is characterized in that: preferably contain 1~3N hydrochloric acid or 1~3N vitriolic, 30%~50% ethanolic soln, degraded 2~5 hours for 100 ℃.
5, method according to claim 1 is characterized in that: top condition is to contain 2N hydrochloric acid or 2N vitriolic 45 ethanolic solns, degrades 3 hours for 100 ℃.
6, the extract according to claim 1 gained is preparing prevention and treatment of diseases medicines such as hyperlipidemia, fatty liver and atheroma.
7, according to the extract of claim 1 gained as the treatment effective amount of actives, and contain one or more pharmaceutically acceptable carriers.
8, medicine according to claim 6 is characterized in that: preferably contain 1%~99% Chinese honey locust triterpenic acid and 99%~1% vehicle.
9, medicine according to claim 6 is characterized in that: contain 10%~90% Chinese honey locust triterpenic acid and 90%~10% pharmaceutical excipient.
10, medicine according to claim 6 is characterized in that: contain 30%~80% Chinese honey locust triterpenic acid and 70%~20% pharmaceutical excipient.
11, medicine according to claim 6 is characterized in that: contain 60%~70% Chinese honey locust triterpenic acid and 40%~30% vehicle.
12, medicine according to claim 6 is characterized in that said medicine is a said formulation on any pharmaceutics.
CNB021098255A 2002-05-22 2002-05-22 Process for extracting triterpenic acid from gleditschia, and medical use and chinese medicine of triterpenic acid Expired - Lifetime CN1169825C (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100395258C (en) * 2003-03-28 2008-06-18 中国医学科学院药用植物研究所 Loquat leaf triterpene acid composition and its uses in preparation of medicine against inflammation and antitussive
CN103145790A (en) * 2013-03-18 2013-06-12 山东省中医药研究院 Method for simultaneously preparing oleanolic acid and echinocystic acid from fructus gleditsiae
CN105111180A (en) * 2015-07-21 2015-12-02 河南科技大学 Method for extraction of new iridoid compound and other compounds from low alcohol spina gleditsiae
CN112007417A (en) * 2020-08-20 2020-12-01 赣州禾绿康健生物技术有限公司 Device and method for removing carbendazim in ganoderma triterpene extract
CN117843280A (en) * 2023-11-28 2024-04-09 四川交通职业技术学院 Concrete early strength agent and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100395258C (en) * 2003-03-28 2008-06-18 中国医学科学院药用植物研究所 Loquat leaf triterpene acid composition and its uses in preparation of medicine against inflammation and antitussive
CN103145790A (en) * 2013-03-18 2013-06-12 山东省中医药研究院 Method for simultaneously preparing oleanolic acid and echinocystic acid from fructus gleditsiae
CN105111180A (en) * 2015-07-21 2015-12-02 河南科技大学 Method for extraction of new iridoid compound and other compounds from low alcohol spina gleditsiae
CN112007417A (en) * 2020-08-20 2020-12-01 赣州禾绿康健生物技术有限公司 Device and method for removing carbendazim in ganoderma triterpene extract
CN117843280A (en) * 2023-11-28 2024-04-09 四川交通职业技术学院 Concrete early strength agent and preparation method thereof

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Address after: No 36, Shu West Road, Chengdu, Sichuan, Jinniu District

Patentee after: Chengdu Kanghong Pharmaceuticals Group Co., Ltd.

Address before: No 36, Shu West Road, Chengdu, Sichuan, Jinniu District

Patentee before: Chengdu Kanghong Sci-Tech Industry (Group) Co., Ltd.

TR01 Transfer of patent right
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Effective date of registration: 20210226

Address after: 611930 No.89 Hualong Road, Tianpeng Town, Pengzhou City, Chengdu City, Sichuan Province

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