CN107970265B - Method for extracting sanchinoside - Google Patents

Method for extracting sanchinoside Download PDF

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Publication number
CN107970265B
CN107970265B CN201711460348.9A CN201711460348A CN107970265B CN 107970265 B CN107970265 B CN 107970265B CN 201711460348 A CN201711460348 A CN 201711460348A CN 107970265 B CN107970265 B CN 107970265B
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extracting
sanchinoside
mixed solution
filtering
esculin
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CN107970265A (en
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马回民
杨青春
胡倩
马怀虎
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Shanghai Zhuangtong Pharmaceutical Technology Co ltd
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Yunnan Hande Bio Tech Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/25Araliaceae (Ginseng family), e.g. ivy, aralia, schefflera or tetrapanax
    • A61K36/258Panax (ginseng)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/55Liquid-liquid separation; Phase separation

Abstract

The invention discloses a method for extracting notoginseng leaf glycoside, which comprises the steps of soaking dried notoginseng stems and leaves in saline solution, extracting, decoloring, recrystallizing and the like to obtain a notoginseng leaf glycoside product with low impurity content.

Description

Method for extracting sanchinoside
Technical Field
The invention relates to an industrial production method for extracting notoginseng leaf glycoside from dried notoginseng stems and leaves.
Background
Pseudo-ginseng is also known as pseudo-ginseng, which is called Jinbuhui by Li Shizhen of famous pharmacologist in the Ming dynasty. The use of notoginseng has a long history. In 1578, the great book of decay of Li Shizhen in Ben Cao gang mu records pseudo-ginseng, which is a golden original drug in south China army and has wonderful work in clouds, and the Chinese patent application records that pseudo-ginseng is just about the beginning of the drug; it is a herb of blood system of yangming jueyin, so it can be used for all kinds of blood diseases. The medicine is known in sea as a specific medicine for traumatic injury, promoting blood circulation and removing blood stasis. In addition to the special efficacy of treating traumatic injury, pseudo-ginseng also has the effects of nourishing and strengthening. Modern pharmacological studies show that the pseudo-ginseng has obvious effects of preventing and treating hyperlipidemia, blood hyperviscosity, hypertension, arrhythmia and the like.
The main active component of the overground part of the panax notoginseng leaf total saponin, namely the panax notoginseng leaf saponin, has the main pharmacological actions of tranquilizing and allaying excitement, easing pain, reducing fat and the like. Has remarkable effect on central nervous system, and can resist exciting effect caused by central stimulant caffeine. The sanchinoside can improve cerebral blood supply, nourish and regulate nerve, restore and coordinate various regulation functions of nervous system, recover physiological sleep to treat neurasthenia, enhance inhibition of cerebral cortex, reduce excitability of subcortical arousal to resist anxiety, and can be used for treating generalized anxiety disorder. Sanchinoside is good for shortening sleep time, prolonging sleep time, reducing wakefulness frequency, and improving headache, dizziness, cardiopalmus, and debilitation.
Blood lipid reducing effect, the esculin can remarkably reduce the content of serum total cholesterol and serum triglyceride, and the effect is related to the panaxadiol saponin component contained in the esculin. As early as 1983, Chinese reported that researchers had already studied sanchinoside, and the documents reported at that time reported that there were seven saponins of sanchinoside, including ginsenoside Rb1, Rb3, Re, 20(R) -ginsenoside-Rg 3, 20(R) -ginsenoside-Rh 2, etc., and gypenoside IX and sanchinoside Fa, Fc and Fe.
Along with the progress of society and the development of science and technology, the requirements of people on living level are higher and higher, the development and the utilization of the sanchinoside are also paid more and more attention, and the sanchinoside has better utilization value in the health care and pharmaceutical industry. Has a high market prospect.
At present, a plurality of methods for extracting the esculin are influenced by the traditional process, and the methods have the defects of complex operation, high input cost, more byproducts, poor color and luster and the like, and are not beneficial to industrial production.
The method for extracting the notoginseng leaf glycoside from the dry notoginseng stems and leaves has the following problems in the prior art or the traditional method:
(1) at present, the method for extracting the notoginseng leaf glycoside from the dry notoginseng stem and leaf mostly adopts water extraction and column chromatography, solvent extraction such as methanol, ethanol or methanol water and ethanol water as extraction solvents; due to the polar nature of the solvents, various impurities of the esculin are extracted together, so that the difficulty is increased for the subsequent column chromatography, and the impurities cannot be effectively controlled; the product quality is reduced, and the extraction cost is increased;
(2) in most of extraction methods reported in the patent documents, necessary column chromatography treatment is required after extraction is finished, and for production enterprises, the column chromatography increases the production period and the production cost; in industrial production, cost control in industrial production is increased.
Disclosure of Invention
The invention aims to provide a method for extracting the sanchinoside, which is clean, low in price, not harsh in extraction conditions, less in byproducts, less in pigment, higher in extraction yield, simple and controllable in method, short in production period and suitable for industrial production of the sanchinoside.
The purpose of the invention is realized by the following technical scheme:
(1) taking dried stem leaves of panax notoginseng as a raw material, heating and soaking the raw material by using a saline solution, filtering, adding the saline solution into filter residues, repeatedly soaking for 1-2 times, combining filtrates, stirring and extracting the filtrate by using petroleum ether, standing for layering, repeatedly extracting a water phase by using the petroleum ether phase for 1 time, and collecting the water phase;
(2) extracting the water phase with n-butanol-isopropanol mixture for 2-3 times, collecting and mixing organic phases, and concentrating the organic phase to obtain crude product of sanchinoside with total saponin content greater than 45%;
(3) dissolving the crude product of the sanchinoside with a methanol-acetone mixed solution by heating, then cooling to-5 to-10 ℃, standing and settling for 12 to 24 hours, filtering, adding a decolorizing agent into the filtrate, carrying out decolorizing treatment at 40 to 45 ℃, filtering, and carrying out rotary evaporation and suction drying on the filtrate to obtain yellow crystal sanchinoside.
Soaking for 4-6 h at 50-60 ℃ in the step (1); the mass concentration of the salt in the salt solution is 5-8%.
The n-butyl alcohol-isopropanol mixed solution is prepared by mixing n-butyl alcohol and isopropanol according to the volume ratio of 4-6: 1.
The methanol-acetone mixed solution is prepared by mixing methanol and acetone according to the volume ratio of 3-5: 1.
The heating temperature in the step (3) is 50-60 ℃.
The decolorizing agent is activated carbon and neutral alumina, the mass ratio of the activated carbon to the neutral alumina is 2-3: 1, and the mass ratio of the crude product of the sanchinoside to the decolorizing agent is 4-6: 1.
The invention has the advantages and technical effects that:
(1) the stem and leaf of Panax notoginseng contain abundant notoginsenoside, ginsenoside, polysaccharide, lipid, chlorophyll, etc.; the invention utilizes the characteristic that the notoginsenoside is well dissolved in water; soaking stem and leaf of Notoginseng radix with water as main solvent; the salt is added to form high osmotic pressure on cells in the stems and leaves of the panax notoginseng so as to realize the rapid extraction of effective components;
(2) adding petroleum ether into the soaked solution for extraction, extracting more than 90% of lipid and pigment, and hardly dissolving the effective components in the petroleum ether, wherein the extraction achieves the primary separation and purification effect;
(3) extracting with n-butanol-isopropanol mixture to separate notoginsenoside and ginsenoside; concentrating to obtain crude product of esculin with total content of effective components greater than 45%;
(4) dissolving the crude product with mixed solution of methanol and acetone, cooling and settling to separate out a large amount of polysaccharide and partial impurities, and decolorizing the filtrate with activated carbon and neutral alumina to obtain arasaponin with total content of effective components greater than 80%.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the invention is not limited to the above-described examples.
Example 1: the method for extracting the esculin comprises the following steps:
(1) adding 5kg of dried folium Notoginseng cut into 1-2cm segments into 50L pan, adding 40L of salt water solution (salt concentration in water is 5%) and heating at 60 deg.C for soaking for 4 hr, filtering, adding 35L of salt water solution with mass concentration of 5% into the filter residue, heating and soaking for 5 hr, and filtering; adding 35L of salt water solution with mass concentration of 5% into the filter residue, heating and soaking for 6 hours, filtering, and combining 105L of the three filtrates;
(2) extraction treatment of saline water immersion liquid and preparation of crude product of notoginseng glycoside
Adding 105L of the filtrate into an extraction tank, adding 21L of petroleum ether (the amount of the petroleum ether is one fifth of the total volume of the filtrate), stirring and extracting, standing for layering, repeatedly extracting the water phase for 1 time by using a petroleum ether phase, and collecting the water phase; separating out a petroleum ether layer, and concentrating and recovering petroleum ether; placing the water phase in an extraction tank, adding 30L of n-butanol-isopropanol mixed solution (volume ratio of n-butanol to isopropanol is 4:1), continuously extracting for 2 times, collecting 55L of combined organic phase, and discharging the water layer into a sewage tank; concentrating and draining the organic phase at 75 deg.C under reduced pressure to obtain 1015g of crude product of sanchinoside, with total saponin content of 37.16% and extraction rate of 7.5%;
(3) preparation of sanchinoside
Heating and dissolving 1015g of crude product of the notoginseng glycoside with 3L of methanol-acetone mixed solution (the methanol-acetone mixed solution is prepared by mixing methanol and acetone according to the volume ratio of 3: 1) at 60 ℃, then cooling to-5 ℃, standing and settling for 20h, filtering, adding 253g of decolorizing agent (the decolorizing agent is active carbon and neutral alumina, the mass ratio of the active carbon to the neutral alumina is 2:1) into the filtrate, placing the filtrate at 40 ℃ for decolorizing treatment for 2h, filtering, performing rotary evaporation and suction drying on the filtrate to obtain 453g of yellow crystal notoginseng glycoside, wherein the checked content of total saponins is 78.8%. The yield thereof was found to be 95.01%.
Example 2: the method for extracting the esculin comprises the following steps:
(1) adding 10kg of dried folium Notoginseng cut into 1-2cm segments into a 100L pan, adding 80L of salt water solution (salt concentration in water is 6%), heating and soaking at 50 deg.C for 6 hr, filtering, adding 70L of salt water solution with mass concentration of 6%, heating and soaking for 5 hr, and filtering; adding 60L of saline solution with the mass concentration of 6% into filter residue, heating and soaking for 6 hours, filtering, and combining the three filtrates 205L;
(2) extraction treatment of saline water immersion liquid and preparation of crude product of notoginseng glycoside
Adding 205L of filtrate into an extraction tank, adding 45L of petroleum ether for extraction, standing for layering, repeatedly extracting the water phase for 1 time by using the petroleum ether phase, and collecting the water phase; placing the water phase in an extraction tank, adding 60L of n-butanol-isopropanol mixed solution (volume ratio of n-butanol to isopropanol is 5:1), continuously extracting for 2 times, collecting 115L of organic phase, and discharging the water layer into a sewage tank; concentrating and draining the organic phase at 75 deg.C under reduced pressure to obtain 2023g of crude product of sanchinoside, with total saponin content of 38.23% and extraction rate of 7.7%;
(3) preparation of sanchinoside
Dissolving 2023g of crude tricresyl in 6L of methanol-acetone mixed solution (the methanol-acetone mixed solution is prepared by mixing methanol and acetone according to the volume ratio of 4:1) at 50 ℃, cooling to-8 ℃, standing and settling for 15h, filtering, adding a decolorizing agent (the decolorizing agent is activated carbon and neutral alumina, the mass ratio of the activated carbon to the neutral alumina is 2.5: 1) 410g (the decolorizing agent is activated carbon and neutral alumina, the mass ratio of the activated carbon to the neutral alumina is 2:1) into the filtrate, carrying out decolorizing treatment at 45 ℃ for 2h, filtering, carrying out rotary evaporation and suction drying on the filtrate to obtain 912.5g of yellow crystal tricresyl, and the detected total saponin content is 77.56%. The yield thereof was found to be 91.5%.
Example 3: the method for extracting the esculin comprises the following steps:
(1) adding 10kg of dried folium Notoginseng cut into 1-2cm segments into a 100L pot, adding 80L of salt water solution (salt with mass concentration of 8% in water), heating and soaking at 55 deg.C for 5 hr, and filtering; adding 70L of 8% salt solution into the filter residue, heating, soaking for 6 hr, and filtering; mixing the filtrates for 2 times;
(2) extraction treatment of saline water immersion liquid and preparation of crude product of notoginseng glycoside
Adding the filtrate into an extraction tank, adding 40L petroleum ether for extraction, standing for layering, repeatedly extracting the water phase with petroleum ether phase for 1 time, and collecting the water phase; placing the water phase in an extraction tank, adding 50L of n-butanol-isopropanol mixed solution (volume ratio of n-butanol to isopropanol is 6:1), continuously extracting for 2 times, collecting organic phase, and discharging water layer into a sewage tank; concentrating and draining the organic phase at 75 deg.C under reduced pressure to obtain crude product of sanchinoside with total saponin content of 35.43% and extraction rate of 7.8%;
(3) preparation of sanchinoside
Dissolving the crude product of the sanchinoside with a methanol-acetone mixed solution 5L of a methanol-acetone mixed solution (the methanol-acetone mixed solution is prepared by mixing methanol and acetone according to a volume ratio of 5:1) at 55 ℃, cooling to-10 ℃, standing and settling for 12h, filtering, adding a decolorizing agent (the decolorizing agent is activated carbon and neutral alumina, the mass ratio of the activated carbon to the neutral alumina is 3: 1) into the filtrate, and the mass ratio of the crude product of the sanchinoside to the decolorizing agent is 6: 1; decolorizing at 43 deg.C for 2 hr, filtering, rotary evaporating the filtrate to obtain yellow crystal of sanchinoside with total saponin content of 79.82%. The yield thereof was found to be 93.47%.

Claims (5)

1. A method for extracting notoginseng leaf glycoside is characterized by comprising the following steps:
(1) taking dried stem leaves of panax notoginseng as a raw material, heating and soaking the raw material by using a saline solution, filtering, adding the saline solution into filter residues, repeatedly soaking for 1-2 times, combining filtrates, stirring and extracting the filtrate by using petroleum ether, standing for layering, repeatedly extracting a water phase by using the petroleum ether phase for 1 time, and collecting the water phase;
(2) extracting the water phase by using a n-butyl alcohol-isopropanol mixed solution for 2-3 times continuously, collecting and combining organic phases, and concentrating the organic phases to obtain a crude product of the sanchinoside;
(3) dissolving the crude product of the sanchinoside with a methanol-acetone mixed solution by heating, then cooling to-5 to-10 ℃, standing and settling for 12 to 24 hours, filtering, adding a decolorizing agent into the filtrate, carrying out decolorizing treatment at 40 to 45 ℃, filtering, and carrying out rotary evaporation and suction drying on the filtrate to obtain yellow crystal sanchinoside;
the mass concentration of the salt in the salt water solution is 5-8%;
the decolorizing agent is activated carbon and neutral alumina, the mass ratio of the activated carbon to the neutral alumina is 2-3: 1, and the mass ratio of the crude product of the sanchinoside to the decolorizing agent is 4-6: 1.
2. The method for extracting esculin according to claim 1, wherein: the n-butyl alcohol-isopropanol mixed solution is prepared by mixing n-butyl alcohol and isopropanol according to the volume ratio of 4-6: 1.
3. The method for extracting esculin according to claim 1, wherein: the methanol-acetone mixed solution is prepared by mixing methanol and acetone according to the volume ratio of 3-5: 1.
4. The method for extracting esculin according to claim 1, wherein: the heating temperature in the step (3) is 50-60 ℃.
5. The method for extracting esculin according to claim 1, wherein: soaking for 4-6 h at 50-60 ℃ in the step (1).
CN201711460348.9A 2017-12-28 2017-12-28 Method for extracting sanchinoside Active CN107970265B (en)

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Publication number Priority date Publication date Assignee Title
CN109134562A (en) * 2018-10-26 2019-01-04 宁县恒瑞康生物科技有限公司 A kind of aesculin purification process

Citations (5)

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Publication number Priority date Publication date Assignee Title
CN1267665A (en) * 1999-03-19 2000-09-27 蓝桂华 Preparation of notoginseng essence as efficient hemostatic material
CN1414009A (en) * 2001-10-26 2003-04-30 香港生物科技研究院 Method for extracting and separating notoginsenoside R1, panaxcoside Re, pseudo-ginseng element from pseudo-ginseng crude powder
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CN1865232A (en) * 2006-06-22 2006-11-22 上海交通大学 Method for extracting notoginseng essence from notoginseng
CN101380472A (en) * 2008-10-27 2009-03-11 秦枫 Use of total saponin from Panax notoginseng stalks and leaves in preparing immunoadjuvants

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1267665A (en) * 1999-03-19 2000-09-27 蓝桂华 Preparation of notoginseng essence as efficient hemostatic material
CN1414009A (en) * 2001-10-26 2003-04-30 香港生物科技研究院 Method for extracting and separating notoginsenoside R1, panaxcoside Re, pseudo-ginseng element from pseudo-ginseng crude powder
WO2006068155A1 (en) * 2004-12-22 2006-06-29 National University Corporation University Of Toyama Agent for reconstructing neural network comprising chinese medicine formulation and method of reconstructing neural network
CN1865232A (en) * 2006-06-22 2006-11-22 上海交通大学 Method for extracting notoginseng essence from notoginseng
CN101380472A (en) * 2008-10-27 2009-03-11 秦枫 Use of total saponin from Panax notoginseng stalks and leaves in preparing immunoadjuvants

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