CN115228583A - Nanometer particle Taxus media wall-broken fine powder and its preparation method - Google Patents

Nanometer particle Taxus media wall-broken fine powder and its preparation method Download PDF

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Publication number
CN115228583A
CN115228583A CN202210922189.4A CN202210922189A CN115228583A CN 115228583 A CN115228583 A CN 115228583A CN 202210922189 A CN202210922189 A CN 202210922189A CN 115228583 A CN115228583 A CN 115228583A
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China
Prior art keywords
vacuum
taxus
powder
nano
fine powder
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CN202210922189.4A
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Chinese (zh)
Inventor
林俊积
王晨宇
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Chengdu Yijun Biotechnology Co ltd
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Chengdu Yijun Biotechnology Co ltd
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Priority to CN202210922189.4A priority Critical patent/CN115228583A/en
Publication of CN115228583A publication Critical patent/CN115228583A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C21/00Disintegrating plant with or without drying of the material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/02Feeding devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/02Cleaning by the force of jets or sprays
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid
    • B08B3/08Cleaning involving contact with liquid the liquid having chemical or dissolving effect

Abstract

The invention provides a nanoparticle taxus media wall-broken fine powder and a preparation method thereof, wherein the preparation method specifically comprises the following steps: step S1, primary crushing, namely crushing the taxus media by using a crusher to ensure that the average particle size of the taxus media reaches 50-100 meshes; s2, performing jet milling, namely milling the taxus chinensis after coarse powder by using a jet mill to ensure that the average particle size of powder particles reaches 350-500 meshes; and S3, nano-grinding, namely grinding the taxus chinensis subjected to jet milling by using a nano grinder to ensure that the average particle size of powder of the taxus chinensis reaches 3000-7000 nanometers. The invention utilizes the most advanced nanoparticle technology to carry out nano-crushing wall breaking, so that the average particle size of powder particles is less than 7000 nanometers, the plant cell walls of the taxus media are completely broken, various nutritional ingredients in the taxus media are completely released, and the utilization rate of the taxus media is greatly improved.

Description

Nanometer particle Taxus media wall-broken fine powder and its preparation method
Technical Field
The invention relates to the technical field of modern pulverization of a high-temperature-solvent-free extraction process, in particular to nano taxus media wall-broken fine powder and a preparation method thereof.
Background
Taxus media is a evergreen shrub of Taxus family introduced from Canada in China, is a natural hybrid variety of artificially cultured Taxus cuspidata and Taxus baccata, is very precious due to high content (0.03% -0.04%) of anticancer specific drug paclitaxel, and is known as "plant gold". Paclitaxel is a natural high-efficiency broad-spectrum anticancer drug with antitumor activity, and can be widely used for treating tumors such as small cell lung cancer, breast cancer, metastatic breast cancer, ovarian cancer, bladder cancer, cervical cancer, late-stage esophageal cancer, gastric cancer, non-small cell lung cancer, etc. Wherein, the paclitaxel has better curative effect on breast cancer, lung cancer, gastric cancer, colorectal cancer, seminoma, recurrent non-Hodgkin lymphoma, brain tumor, head and neck cancer and the like, and particularly has extremely obvious curative effect on the treatment of advanced ovarian cancer and postoperative rehabilitation of patients with general postoperative cancers. The PDB and the data of the safety securities institute show that: paclitaxel accounts for a large proportion of its sample hospital antineoplastic drug sales. Besides paclitaxel, taxus media also contains various alkaloids, diterpenoid compounds and other substances beneficial to human body, and has remarkable curative effects on insomnia, warming kidney, dredging channels, reducing weight, enhancing immunity, reducing blood sugar, resisting radiation, cardiovascular diseases and the like.
At present, the phenomenon of wasting medicinal beneficial components exists in the process of paclitaxel extraction of taxus media, and products such as high-purity paclitaxel injection and the like are high in price, so that common people cannot bear the medicament cost easily.
Disclosure of Invention
In order to solve the technical problems of low development and utilization efficiency and serious waste of the taxus media in the prior art, the preparation method of the nano-particle taxus media wall-broken fine powder provided by the invention specifically comprises the following steps:
step S1, primary crushing, namely crushing the taxus media by using a crusher to ensure that the average particle size of the taxus media reaches 50-100 meshes;
s2, performing jet milling, namely milling the taxus chinensis after coarse powder by using a jet mill to ensure that the average particle size of powder particles reaches 350-500 meshes;
and S3, nano-grinding, namely grinding the taxus chinensis subjected to jet milling by using a nano grinder to ensure that the average particle size of powder of the taxus chinensis reaches 3000-7000 nanometers.
Further, the step S1 specifically includes the following steps:
step S11, preprocessing, namely cleaning fresh barks, branches and leaves and roots of Chinese yew, naturally drying, crushing by using a crusher, sieving by using a 80-mesh sieve to obtain fine powder, and then performing vacuum drying on the fine powder to obtain powder;
and S12, neutralizing and detoxifying, adding acetic acid with three times of volume into the powder for soaking, performing vacuum filtration, performing acetic acid leaching on the filter residue for 2 times by the same method, adding deionized water with two times of volume into the filter residue obtained by the last filtration for soaking, performing water leaching on the residue obtained by the vacuum filtration for 2 times by the same method, and performing vacuum drying on the obtained residue.
Further, in the step S11, picking up the bark, branches and leaves and roots of the fresh yew of more than 5 years old, cleaning dust and dirt on the surface with clear water, circularly rinsing with a weak acid detergent, rinsing with clear water, finally spraying with deionized water, naturally drying the cleaned bark, branches and leaves and roots of the yew, crushing with a crusher, sieving with a 80-mesh sieve to obtain fine powder, and then vacuum drying the fine powder to obtain the powder.
Further, in the step S12, acetic acid with a mass concentration of 2% is added to be soaked for 2 hours at 33 ℃, the usage amount of the acetic acid is three times of the volume of the powder, vacuum filtration is performed after the acetic acid soaking, the filter residue obtained by the filtration is leached for 2 times with the acetic acid by the same method, deionized water with a volume which is two times of the filter residue obtained by the last filtration is added to the filter residue obtained by the last filtration, after the filter residue is soaked for 2 hours at 36 ℃, the residue obtained by the vacuum filtration is leached for 2 times with the same method, and then the residue obtained finally is dried in vacuum.
Further, the specific conditions of the vacuum drying are 40 ℃, vacuum degree: 0.08 to 0.10MPa.
Further, in the step S2, the jet mill may be a jet mill, a flat jet mill, a circulating tube jet mill, or a fluidized bed jet mill.
Further, in the step S3, the nano grinder includes a vacuum hopper, a vacuum screw feeder, a vacuum feed pipe, a vacuum collection bin, a rotating wheel and a grinding ring in the vacuum collection bin.
Further, after the crushed materials are placed into a vacuum charging hopper, the materials are uniformly distributed to the outer end parts of the shells by the rotation of screws in a horizontally-distributed vacuum spiral feeder in a vacuum state, the materials are enabled to freely and quickly fall into the upper part of a vacuum collecting bin in the vacuum state through a vertically-distributed vacuum conveying pipe below a discharge port of the outer end part, namely, the materials are impacted and instantaneously crushed by a rotating wheel rotating at a high speed, crushed particles are thrown to a grinding ring fixed on the inner wall of the collecting bin at a high speed relative to the height position of the rotating wheel under the action of centrifugal force, and are further crushed, the particles crushed twice fall into a discharge port at the bottom of the collecting bin, are received by a set container, then return to the vacuum charging hopper at the top for repeated crushing, and are taken out after a system is closed to release vacuum until the expected nanometer size is obtained.
The nano-particle taxus media wall-broken fine powder provided by the invention is prepared by adopting the preparation method, and insoluble beneficial ingredients contained in the taxus media are converted into stable nano-particle particles, so that the nano-particle taxus media wall-broken fine powder is convenient to take orally and inject and absorb.
Compared with the prior art, the invention has the following beneficial effects:
the invention takes Taxus media as raw material, utilizes the most advanced nanoparticle technology and a physical method, and utilizes a composite force field formed by special shearing to carry out nano crushing wall breaking, so that the average particle size of powder particles is less than 7000 nanometers, the plant cell wall of the Taxus media is completely broken, various nutritional ingredients are completely released, and the utilization degree of the Taxus media is greatly improved.
Drawings
Fig. 1 is a flow chart of a preparation method of nano taxus media wall-broken fine powder in the embodiment of the invention.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, embodiments of the present invention will now be described with reference to the accompanying drawings.
As shown in fig. 1, the preparation method of the nano taxus media wall-broken fine powder provided by the embodiment of the invention specifically comprises the following steps:
and step S1, primarily crushing, namely crushing the Taxus media by using a crusher to ensure that the average particle size of the Taxus media reaches 50-100 meshes. The method comprises the following specific steps:
step S11, preprocessing, cleaning fresh barks, branches and leaves and roots of Chinese yew, naturally drying, crushing by a crusher, sieving by an 80-mesh sieve to obtain fine powder, then carrying out vacuum drying on the fine powder to obtain powder, specifically, picking fresh barks, branches and leaves and roots of Chinese yew of more than 5 years old, washing dust and dirt on the surface by clear water, circularly leaching by weak acid detergent, leaching by clear water, finally spraying and washing by deionized water, naturally drying the cleaned barks, branches and leaves and roots of Chinese yew, crushing by the crusher, sieving by the 80-mesh sieve to obtain fine powder, and carrying out vacuum drying on the fine powder at 40 ℃ under the condition that the vacuum degree is 0.08-0.10 Mpa to obtain powder.
S12, neutralizing and detoxifying, adding acetic acid with three times of volume into the powder for soaking, performing vacuum filtration, performing acetic acid leaching on the filter residue for 2 times by the same method, adding deionized water with two times of volume into the filter residue obtained by the last filtration for soaking, performing vacuum filtration on the residue obtained by the vacuum filtration for 2 times by the same method, performing vacuum drying on the obtained residue, specifically, adding acetic acid with the mass concentration of 2% for soaking for 2 hours at 33 ℃, wherein the usage amount of the acetic acid is three times of the volume of the powder, performing vacuum filtration after soaking the acetic acid, leaching the filter residue obtained by the filtration for 2 times by the same method, adding deionized water with two times of volume into the filter residue obtained by the last filtration, soaking for 2 hours at 36 ℃, performing vacuum filtration on the obtained residue for 2 times by the same method, and performing vacuum drying on the residue obtained by the last filtration at 40 ℃ under the vacuum degree of 0.08-0.10 MPa.
And S2, performing jet milling, namely milling the taxus chinensis after coarse powder by using a jet mill to ensure that the average particle size of powder particles reaches 350-500 meshes. The jet mill uses supersonic speed high turbulence air flow generated by compressed air or superheated steam through a nozzle as a carrier of particles, and impact extrusion friction and shearing and the like are generated between the particles or between the particles and a fixed plate, so that the purpose of crushing is achieved. The jet mill can be selected from a counter-jet mill, a flat jet mill, a circulating tube jet mill or a fluidized bed jet mill.
And S3, nano-grinding, namely grinding the taxus chinensis subjected to jet milling by using a nano grinder to ensure that the average particle size of powder of the taxus chinensis reaches 3000-7000 nanometers. The nano crusher includes vacuum material feeding bin, vacuum spiral material feeder, vacuum material conveying pipes, vacuum material collecting bin, rotating wheels and grinding rings inside the vacuum material collecting bin.
The nanoparticle taxus media wall-broken fine powder provided by the embodiment of the invention is prepared by the preparation method, can be processed and extracted again, can be directly used as raw materials of medical appliances, health products, foods, medicines and the like, reduces the extraction difficulty, and can achieve the purpose of fully utilizing beneficial ingredients of the taxus media and enabling the beneficial ingredients to directly enter focuses.
The invention takes Taxus media as raw material, utilizes the most advanced nanoparticle technology and a physical method, and utilizes a composite force field formed by special shearing to carry out nano crushing wall breaking, so that the average particle size of powder particles is less than 7000 nanometers, the plant cell wall of the Taxus media is completely broken, various nutritional ingredients are completely released, and the utilization degree of the Taxus media is greatly improved. The invention can convert insoluble beneficial components which are difficult to be extracted, such as paclitaxel and the like contained in the taxus media into stable nanoparticle particles, and is more convenient for oral administration and injection absorption.
Compared with the prior art, the invention has the following remarkable advantages:
1) The product is processed by using a jet milling method without multiple refining and extraction in the processing process, so that the quality stability of the product is ensured;
2) The root, the stem, the leaf, the trunk and the bark of the taxus chinensis are fully utilized in the processing process, so that the raw material resources are saved, the production cost is reduced, and the method is beneficial to the common people.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and should not be taken as limiting the scope of the present invention. It should be noted that those skilled in the art should recognize that they may make equivalent variations to the embodiments of the present invention without departing from the spirit and scope of the present invention.

Claims (9)

1. The preparation method of the nano taxus media wall-broken fine powder is characterized by comprising the following steps:
step S1, primarily crushing, namely crushing Taxus media by using a crusher to enable the average particle size of the Taxus media to reach 50-100 meshes;
s2, performing jet milling, namely milling the taxus chinensis after coarse powder by using a jet mill to ensure that the average particle size of powder particles reaches 350-500 meshes;
and S3, nano-grinding, namely grinding the taxus chinensis subjected to jet milling by using a nano grinder to ensure that the average particle size of the powder reaches 3000-7000 nanometers.
2. The preparation method according to claim 1, wherein the step S1 specifically comprises the steps of:
step S11, preprocessing, namely cleaning fresh barks, branches and leaves and roots of Chinese yew, naturally drying the barks, the branches and leaves and the roots of the Chinese yew, crushing the barks, the branches and the leaves and the roots of the Chinese yew by using a crusher, sieving the barks and the roots of the Chinese yew by using a 80-mesh sieve to obtain fine powder, and then performing vacuum drying on the fine powder to obtain powder;
and S12, neutralizing and detoxifying, adding acetic acid with three times of volume into the powder for soaking, performing vacuum filtration, performing acetic acid leaching on the filter residue for 2 times by the same method, adding deionized water with two times of volume into the filter residue obtained by the last filtration for soaking, performing water leaching on the residue obtained by the vacuum filtration for 2 times by the same method, and performing vacuum drying on the obtained residue.
3. The method according to claim 2, wherein in step S11, the bark, branches and leaves, and roots of 5 years old or more of fresh yew are picked up, the surface of the bark, branches and leaves is cleaned with clean water, then the bark, branches and leaves are rinsed with weak acidic detergent in a circulating manner, then rinsed with clean water, finally the bark, branches and leaves are rinsed with deionized water, the cleaned bark, branches and leaves, and roots of yew are naturally dried, then the bark, branches and leaves are pulverized by a pulverizer, fine powder is sieved out with an 80-mesh sieve, and then the fine powder is vacuum-dried to obtain powder.
4. The preparation method according to claim 2, wherein in step S12, acetic acid with a mass concentration of 2% is added and soaked for 2 hours at 33 ℃, the usage amount of the acetic acid is three times of the powder volume, vacuum filtration is performed after the acetic acid soaking, the filter residue obtained by the filtration is leached for 2 times with the acetic acid by the same method, deionized water with a volume twice of the filter residue obtained by the last filtration is added to the filter residue obtained by the last filtration, and after the filter residue is soaked for 2 hours at 36 ℃, the residue obtained by the vacuum filtration is leached for 2 times with the same method, and then the residue obtained is vacuum-dried.
5. The production method according to any one of claims 2 to 4, wherein the specific conditions of the vacuum drying are 40 ℃, vacuum degree: 0.08 to 0.10MPa.
6. The method according to claim 1, wherein in the step S2, the jet mill is selected from a counter-jet type jet mill, a flat type jet mill, a circulating tube type jet mill, and a fluidized bed type jet mill.
7. The method as set forth in claim 1, wherein in the step S3, the nano-pulverizer includes a vacuum hopper, a vacuum screw feeder, a vacuum feed pipe, a vacuum collection bin, a rotating wheel and a grinding ring in the vacuum collection bin.
8. The preparation method of claim 7, wherein after the pulverized material is placed in the vacuum hopper, the material is uniformly distributed to the outer end of each shell by the rotation of the screws in the horizontally arranged vacuum screw feeder under vacuum, the material is freely accelerated and falls into the upper part of the vacuum aggregate bin under vacuum through the vertically arranged vacuum delivery pipe from the lower part of the discharge port at the outer end, namely, the material is impacted and instantly pulverized by the rotating wheel rotating at high speed, the pulverized particles are thrown to the grinding ring fixed on the inner wall of the aggregate bin at high speed relative to the height position of the rotating wheel under the centrifugal force, and then are further pulverized, the particles pulverized twice fall into the discharge port at the bottom of the aggregate bin, are received by the set container, then return to the vacuum hopper at the top for repeated pulverization, and are taken out after the vacuum of the closed system is released after the expected nanometer size is obtained.
9. The nano taxus media wall-broken fine powder is characterized by being prepared by the preparation method of any one of claims 1 to 8, and insoluble beneficial ingredients contained in taxus media are converted into stable nano particles, so that the nano taxus media wall-broken fine powder is convenient to take orally and inject and absorb.
CN202210922189.4A 2022-08-02 2022-08-02 Nanometer particle Taxus media wall-broken fine powder and its preparation method Pending CN115228583A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2790583Y (en) * 2005-05-20 2006-06-28 宁波西科蒙特钻石有限公司 Dry vacuum nano disintegrating machine
CN101837029A (en) * 2009-03-19 2010-09-22 粟时献 Nanometer taxus chinensis powder and preparation method thereof
CN102813682A (en) * 2012-07-19 2012-12-12 李振刚 Stir-frying technology for Chinese yew powder rich in paclitaxel liposome by using membrane-ultrasonic wave dissolving technique
CA2774862A1 (en) * 2012-04-23 2013-10-23 Xiao Huanping Pulverizer
CN107961253A (en) * 2017-12-05 2018-04-27 陕西省西安植物园 A kind of Taxus extracts through detoxification treatment and preparation method thereof
CN109833335A (en) * 2017-11-29 2019-06-04 粟时献 Nano-taxus thimerosal and preparation method thereof
CN111760669A (en) * 2020-07-02 2020-10-13 无锡紫杉药业有限公司 Method for screening raw materials for producing paclitaxel

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2790583Y (en) * 2005-05-20 2006-06-28 宁波西科蒙特钻石有限公司 Dry vacuum nano disintegrating machine
CN101837029A (en) * 2009-03-19 2010-09-22 粟时献 Nanometer taxus chinensis powder and preparation method thereof
CA2774862A1 (en) * 2012-04-23 2013-10-23 Xiao Huanping Pulverizer
CN102813682A (en) * 2012-07-19 2012-12-12 李振刚 Stir-frying technology for Chinese yew powder rich in paclitaxel liposome by using membrane-ultrasonic wave dissolving technique
CN109833335A (en) * 2017-11-29 2019-06-04 粟时献 Nano-taxus thimerosal and preparation method thereof
CN107961253A (en) * 2017-12-05 2018-04-27 陕西省西安植物园 A kind of Taxus extracts through detoxification treatment and preparation method thereof
CN111760669A (en) * 2020-07-02 2020-10-13 无锡紫杉药业有限公司 Method for screening raw materials for producing paclitaxel

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Application publication date: 20221025