CN107435060A - A kind of preparation method of longan nuclear protein polypeptide - Google Patents
A kind of preparation method of longan nuclear protein polypeptide Download PDFInfo
- Publication number
- CN107435060A CN107435060A CN201710907944.0A CN201710907944A CN107435060A CN 107435060 A CN107435060 A CN 107435060A CN 201710907944 A CN201710907944 A CN 201710907944A CN 107435060 A CN107435060 A CN 107435060A
- Authority
- CN
- China
- Prior art keywords
- longan
- longan seed
- solution
- ultramicro
- nuclear protein
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P21/00—Preparation of peptides or proteins
- C12P21/06—Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biotechnology (AREA)
- Molecular Biology (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention relates to a kind of preparation method of longan nuclear protein polypeptide, belong to food technology field.The preparation method of the longan nuclear protein polypeptide, comprises the following steps:S1. crush:Longan seed is dried, ultramicro grinding, longan seed Ultramicro-powder is made;S2. extract:According to mass volume ratio it is 1 by longan seed Ultramicro-powder obtained by step S1 and water:8 12 dissolvings, adjust pH to 9 11, using ultrasonic microwave combined extracting, filtering, obtain extract solution, extract solution is precipitated using isoelectric point ethanol co precipitation method, vacuum drying, obtains longan nucleoprotein;S3. activated carbon decolorizing;S4. digest:The longan seed protein solution regulation pH value that step S3 is obtained is 7.2 7.6, enzymolysis, after enzymolysis, enzyme deactivation, filters, concentration, dries and longan nuclear protein polypeptide is made.The method of the invention recovery rate is high, and technique is simple, easy to operate, and cost is cheap, is adapted to industrialized production.
Description
【Technical field】
The present invention relates to food technology field, and in particular to a kind of preparation method of longan nuclear protein polypeptide.
【Background technology】
With the development of people's living standards continue to improve and modern nutriology, people recognize to take in excessive richness further
Food containing animal protein may bring the health problems such as high fat of blood, high cholesterol.By contrast, vegetable protein has
The advantages that low cholesterol and high protein, it is relatively beneficial to health.Vegetable protein beverage is nutritious, can provide needed by human body
Proteins,vitamins,and minerals etc., also tend to that there is certain health-care effect due to functional components specific to raw material.
Analysis display, the coming five years, China will adjust beverage industry structure, while continuing to improve production, give priority to fruit
The products such as vegetable juice beverage, vegetable protein beverage and tea beverage, the ratio of the carbonated beverages such as cola is reduced, develop simultaneously standard function
The production of property beverage.
Longan nucleoprotein is a kind of higher vegetable protein of nutritive value, and it contains 8 kinds of essential amino acids of needed by human body,
Easily digested and assimilated for human body, to safeguarding that health and early children development play an important roll.And longan nucleoprotein is made through digesting
Longan seed polypeptide can directly be absorbed without degraded by enteron aisle, infiltration rate and absorptivity ratio protein and amino acid are all high, and also
With health cares such as the growth metabolisms of profitable strain such as reducing blood lipid, norcholesterol, anti-oxidant, raising immunity, promotion Bifidobacterium
Effect.
Therefore, prepare a kind of longan nuclear protein polypeptide using longan seed and will be provided with good market prospects.
【The content of the invention】
The goal of the invention of the present invention is:For above-mentioned problem, there is provided a kind of preparation of longan nuclear protein polypeptide
Method, methods described recovery rate is high, and technique is simple, easy to operate, and cost is cheap, is adapted to industrialized production.
To achieve these goals, the technical solution adopted by the present invention is as follows:
A kind of preparation method of longan nuclear protein polypeptide, comprises the following steps:
S1. crush:Longan seed is dried, ultramicro grinding, longan seed Ultramicro-powder is made;
S2. extract:According to mass volume ratio it is 1 by longan seed Ultramicro-powder obtained by step S1 and water:8-12 dissolves, and adjusts pH
To 9-11, using ultrasonic-microwave combined extracting, filtering, extract solution is obtained, extract solution uses isoelectric point-ethanol co precipitation
Method precipitates, and vacuum drying, obtains longan nucleoprotein;
S3. activated carbon decolorizing:The longan nucleoprotein that step S2 is obtained is added into water, regulation pH value to 4.0 is made into quality volume
Fraction is 8-12% solution, adds activated carbon, and the addition of activated carbon needs 1g activated carbons to calculate by every 100ml solution, filtering,
Obtain longan seed protein solution;
S4. digest:It is 7.2-7.6 by the longan seed protein solution regulation pH value that step S3 is obtained, enzymolysis, enzymolysis finishes
Afterwards, enzyme deactivation, filter, concentration, dry and longan nuclear protein polypeptide is made.
Further, in step S1, the ultramicro grinding is that the average grain diameter of longan seed Ultramicro-powder after crushing is 10~20 μ
m。
Further, in step S2, the ultrasonic-microwave combined extracting is to be in 60-70 DEG C of temperature, ultrasonic power
6-8min is extracted under 150-200W, microwave power 300w.
Further, in step S3, the condition of the activated carbon decolorizing is:80 DEG C of temperature, bleaching time 40min.
Further, in step S4, the enzymolysis is is 55-60 DEG C in temperature, under conditions of ultrasonic wave 70W, by 0.8g/
100ml-1g/100ml adds alkali protease, is hydrolyzed by 0.5g/100ml addition calcium chloride into the longan seed protein solution
After 2h-3h, then by 0.4g/100ml-0.6g/100ml addition compound fertilizer production hydrolysis 2h-3h.
Preferably, in step S4, the weight proportion of the alkali protease and the compound fertilizer production is 2:1.
Present invention additionally comprises the longan nuclear protein polypeptide that the above method is prepared.
In summary, by adopting the above-described technical solution, the beneficial effects of the invention are as follows:
(1) present invention uses ultrasonic-microwave combined extracting, can not only retain longan nucleoprotein to greatest extent, and
And the recovery rate of longan nucleoprotein can be improved, while shorten extraction time.
(2) extract solution of the present invention is using isoelectric point-ethanol co precipitation method precipitation, and rate of deposition is higher, the time required to precipitation
It is shorter.
(3) present invention is under ultrasonic wave and zymoexciter synergy, using two kinds of protease (alkali protease and compound
Flavor protease) double enzymolysis method, protein hydrolysis degree and polypeptide yield are high.
(4) preparation method technique of the invention is simple, and easy to operate, time saving and cost is cheap, is adapted to industrialized production.
【Embodiment】
Embodiment 1
A kind of preparation method of longan nuclear protein polypeptide, comprises the following steps:
S1. crush:Longan seed is dried, ultramicro grinding, the longan seed Ultramicro-powder that average grain diameter is 10~20 μm is made;
S2. extract:According to mass volume ratio it is 1 by longan seed Ultramicro-powder obtained by step S1 and water:10 dissolving, regulation pH to
10, using ultrasonic-microwave combined extracting, extracted at 65 DEG C, ultrasonic power 150-200W, microwave power 300w of temperature
6min, filtering obtain extract solution, and extract solution vacuum drying, obtains longan seed using isoelectric point-ethanol co precipitation method precipitation
Albumen;
S3. activated carbon decolorizing:The longan nucleoprotein that step S2 is obtained is added into water, regulation pH value to 4.0 is made into quality volume
Fraction is 10% solution, adds activated carbon, the addition of activated carbon needs 1g activated carbons to calculate by every 100ml solution, in temperature
Under conditions of 80 DEG C, bleaching time 40min, filtering, longan seed protein solution is obtained;
S4. digest:It is 7.2-7.6 by the longan seed protein solution regulation pH value that step S3 is obtained, is 55-60 in temperature
DEG C, under conditions of ultrasonic wave 70W, alkali protease is added by 0.8g/100ml, calcium chloride is added to described by 0.5g/100ml
After hydrolyzing 2h in longan seed protein solution, then by 0.4g/100ml addition compound fertilizer production hydrolysis 2h, after enzymolysis, go out
Enzyme, filter, longan nuclear protein polypeptide is made in concentration, freeze-drying.
Embodiment 2
A kind of preparation method of longan nuclear protein polypeptide, comprises the following steps:
S1. crush:Longan seed is dried, ultramicro grinding, the longan seed Ultramicro-powder that average grain diameter is 10~20 μm is made;
S2. extract:According to mass volume ratio it is 1 by longan seed Ultramicro-powder obtained by step S1 and water:8 dissolving, regulation pH to
9, using ultrasonic-microwave combined extracting, extracted under temperature 60 C, ultrasonic power 150-200W, microwave power 300w
8min, filtering obtain extract solution, and extract solution vacuum drying, obtains longan seed using isoelectric point-ethanol co precipitation method precipitation
Albumen;
S3. activated carbon decolorizing:The longan nucleoprotein that step S2 is obtained is added into water, regulation pH value to 4.0 is made into quality volume
Fraction is 8% solution, adds activated carbon, and the addition of activated carbon needs 1g activated carbons to calculate, is in temperature by every 100ml solution
Under conditions of 80 DEG C, bleaching time 40min, filtering, longan seed protein solution is obtained;
S4. digest:It is 7.2-7.6 by the longan seed protein solution regulation pH value that step S3 is obtained, is 55-60 in temperature
DEG C, under conditions of ultrasonic wave 70W, alkali protease is added by 1g/100ml, calcium chloride is added to the dragon by 0.5g/100ml
After hydrolyzing 3h in eye nucleoprotein solution, then by 0.4g/100ml addition compound fertilizer production hydrolysis 2h, after enzymolysis, go out
Enzyme, filter, longan nuclear protein polypeptide is made in concentration, freeze-drying.
Embodiment 3
A kind of preparation method of longan nuclear protein polypeptide, comprises the following steps:
S1. crush:Longan seed is dried, ultramicro grinding, the longan seed Ultramicro-powder that average grain diameter is 10~20 μm is made;
S2. extract:According to mass volume ratio it is 1 by longan seed Ultramicro-powder obtained by step S1 and water:12 dissolving, regulation pH to
11, using ultrasonic-microwave combined extracting, extracted under temperature 70 C, ultrasonic power 150-200W, microwave power 300w
7min, filtering obtain extract solution, and extract solution vacuum drying, obtains longan seed using isoelectric point-ethanol co precipitation method precipitation
Albumen;
S3. activated carbon decolorizing:The longan nucleoprotein that step S2 is obtained is added into water, regulation pH value to 4.0 is made into quality volume
Fraction is 12% solution, adds activated carbon, the addition of activated carbon needs 1g activated carbons to calculate by every 100ml solution, in temperature
Under conditions of 80 DEG C, bleaching time 40min, filtering, longan seed protein solution is obtained;
S4. digest:It is 7.2-7.6 by the longan seed protein solution regulation pH value that step S3 is obtained, is 55-60 in temperature
DEG C, under conditions of ultrasonic wave 70W, alkali protease is added by 0.8g/100ml, calcium chloride is added to described by 0.5g/100ml
After hydrolyzing 2h in longan seed protein solution, then by 0.6g/100ml addition compound fertilizer production hydrolysis 3h, after enzymolysis, go out
Enzyme, filter, longan nuclear protein polypeptide is made in concentration, freeze-drying.
Experimental example 1:The comparison of longan nucleoprotein ultrasonic-microwave combined extracting and other method
Ultrasonic-microwave combined extracting and microwave radiation exaraction, ultrasound assisted extraction, the extraction of conventional heating water bath are carried out
Compare, as a result such as table 1.
The comparison of the Different Extraction Method of table 1
As can be seen from the above table, ultrasonic-microwave combined extracting of the invention and other extracting method ratios, there is extraction effect
The advantages that rate is high, extraction time is short and DNA purity is high.
The quality of the quality of protein/longan seed Ultramicro-powder total protein in longan seed protein extracting ratio (%)=extract solution ×
100%.
By extract solution protein precipitation, after freeze-drying, the quality of albumen in extract is determined with Coomassie Brilliant Blue, is calculated
Longan seed purity of protein, quality × 100% of quality/extract of albumen in purity of protein (%)=extract.
Experimental example 2:The selection of longan seed albumen precipitation method
Extract solution obtained by ultrasonic-microwave combined extracting is respectively taken into 5ml, isoelectric point precipitation, tetraploid is respectively adopted
After the product absolute ethyl alcohol precipitation method and isoelectric point ethanol co precipitation method precipitation, vacuum freeze drying, longan seed albumen precipitation is calculated
Rate, it is compared, is shown in Table 2.
The selection of the longan seed albumen precipitation method of table 2
Project | The time required to precipitation (min) | Rate of deposition (%) |
Isoelectric point precipitation | 5-8 | 80.3 |
Ethanol precipitation | 120-220 | 93.5 |
Isoelectric point-ethanol co precipitation method | 5-8 | 98.6 |
As can be seen from the above table, the intermediate processing of present invention selection selection isoelectric point ethanol synergy, the electricity such as combine
The advantages of point settling velocity is fast, and alcohol precipitation is complete, rate of deposition can be made to reach 98.6%, be only 5 minutes the time required to precipitation.
Albumen quality × 100% in albumen quality/extract solution of longan seed albumen precipitation rate (%)=precipitation.
Experimental example 3:The screening of protease
On the basis of alkali protease and the single enzyme hydrolysis of compound fertilizer production, in order to reach higher degree of hydrolysis,
Using ultrasonic wave and the lower alkali protease of zymoexciter synergy and compound fertilizer production double enzymolysis method, first basic protein
Enzyme digests, rear compound fertilizer production enzymolysis, as a result such as table 3.
3 single enzyme of table and double enzyme enzymolysis process effects compare
As can be seen from the above table, alkali protease enzymolysis gained longan nuclear protein polypeptide degree of hydrolysis is minimum, composite flavor egg
The longan nuclear protein polypeptide degree of hydrolysis of white enzyme enzymolysis gained is 26.7%, higher than alkali protease.But through alkali protease and again
The degree of hydrolysis for closing sequential hydrolysis after flavor protease compounds significantly improves, and through ultrasonic wave and zymoexciter lower pair of enzyme of synergy
The degree of hydrolysis highest of method of double crossing enzymolysis.Therefore this experiment determine longan seed proteolysis final technique be defined as ultrasonic wave with
Under zymoexciter synergy, first with the double enzyme method of double crossing hydrolyzed after hydrolysis by novo with compound fertilizer production.
The measure of degree of hydrolysis (DH) of the present invention uses pH-Star methods.
Described above is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair
Bright patent claim, the equal change completed or modification change under the technical spirit suggested by all present invention, all should belong to
Cover the scope of the claims in the present invention.
Claims (7)
1. a kind of preparation method of longan nuclear protein polypeptide, it is characterised in that comprise the following steps:
S1. crush:Longan seed is dried, ultramicro grinding, longan seed Ultramicro-powder is made;
S2. extract:According to mass volume ratio it is 1 by longan seed Ultramicro-powder obtained by step S1 and water:8-12 dissolves, and adjusts pH to 9-
11, using ultrasonic-microwave combined extracting, filtering, extract solution is obtained, extract solution is sunk using isoelectric point-ethanol co precipitation method
Form sediment, vacuum drying, obtain longan nucleoprotein;
S3. activated carbon decolorizing:The longan nucleoprotein that step S2 is obtained is added into water, regulation pH value to 4.0 is made into quality volume fraction
For 8-12% solution, activated carbon is added, the addition of activated carbon needs 1g activated carbons to calculate, filtering, obtained by every 100ml solution
Longan seed protein solution;
S4. digest:It is 7.2-7.6 by the longan seed protein solution regulation pH value that step S3 is obtained, digests, after enzymolysis, go out
Enzyme, filter, concentration, dry and longan nuclear protein polypeptide is made.
2. according to the method for claim 1, it is characterised in that in step S1, the ultramicro grinding is longan seed after crushing
The average grain diameter of Ultramicro-powder is 10~20 μm.
3. according to the method for claim 1, it is characterised in that in step S2, the ultrasonic-microwave combined extracting be
60-70 DEG C of temperature, 6-8min is extracted under ultrasonic power 150-200W, microwave power 300w.
4. according to the method for claim 1, it is characterised in that in step S3, the condition of the activated carbon decolorizing is:Temperature
80 DEG C, bleaching time 40min.
5. according to the method for claim 1, it is characterised in that it is described to digest to be 55-60 DEG C in temperature in step S4,
Under conditions of ultrasonic wave 70W, alkali protease is added by 0.8g/100ml-1g/100ml, calcium chloride is added by 0.5g/100ml
After 2h-3h being hydrolyzed into the longan seed protein solution, then by 0.4g/100ml-0.6g/100ml addition compound fertilizer productions
Hydrolyze 2h-3h.
6. according to the method for claim 5, it is characterised in that in step S4, the alkali protease and the compound wind
The weight proportion of taste protease is 2:1.
7. the longan nuclear protein polypeptide that any one of claim 1-6 methods described is prepared.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710907944.0A CN107435060B (en) | 2017-09-29 | 2017-09-29 | Preparation method of longan nucleoprotein polypeptide |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201710907944.0A CN107435060B (en) | 2017-09-29 | 2017-09-29 | Preparation method of longan nucleoprotein polypeptide |
Publications (2)
Publication Number | Publication Date |
---|---|
CN107435060A true CN107435060A (en) | 2017-12-05 |
CN107435060B CN107435060B (en) | 2021-02-09 |
Family
ID=60461964
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201710907944.0A Active CN107435060B (en) | 2017-09-29 | 2017-09-29 | Preparation method of longan nucleoprotein polypeptide |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107435060B (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108517341A (en) * | 2018-04-23 | 2018-09-11 | 西安德氏禾本生物科技有限公司 | A kind of preparation process of elastin laminin |
CN110951809A (en) * | 2019-09-04 | 2020-04-03 | 内蒙古立泰锐晟智能科技有限公司 | Process for preparing quinoa wheat polypeptide powder |
CN113372409A (en) * | 2021-06-08 | 2021-09-10 | 山东农业工程学院 | Method for extracting tenebrio molitor protein by ultrafine grinding-ultrasonic wave-microwave coupling |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102845585A (en) * | 2012-09-20 | 2013-01-02 | 陕西师范大学 | Polyethylene glycol-microwave assisted almond protein extraction method |
CN104177508A (en) * | 2014-08-06 | 2014-12-03 | 南昌大学 | Method for comprehensively extracting tea seed saponin, tea seed polypeptide and tea seed polysaccharide from tea seed cake |
EP2902034A1 (en) * | 2012-09-28 | 2015-08-05 | Joben Bio-Medical Co., Ltd. | Use of longan seed alcohol extract |
-
2017
- 2017-09-29 CN CN201710907944.0A patent/CN107435060B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102845585A (en) * | 2012-09-20 | 2013-01-02 | 陕西师范大学 | Polyethylene glycol-microwave assisted almond protein extraction method |
EP2902034A1 (en) * | 2012-09-28 | 2015-08-05 | Joben Bio-Medical Co., Ltd. | Use of longan seed alcohol extract |
CN104177508A (en) * | 2014-08-06 | 2014-12-03 | 南昌大学 | Method for comprehensively extracting tea seed saponin, tea seed polypeptide and tea seed polysaccharide from tea seed cake |
Non-Patent Citations (4)
Title |
---|
吴菲菲等: "超声技术在食品工业中的研究应用", 《食品安全质量检测学报》 * |
周玲玲: "玉米花生复合蛋白酶解产物生物活性及加工性能的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
孙君社等: "《现代食品加工学》", 28 February 2001 * |
梅星元等: "《生物化学》", 31 August 2007, 华中师范大学出版社 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108517341A (en) * | 2018-04-23 | 2018-09-11 | 西安德氏禾本生物科技有限公司 | A kind of preparation process of elastin laminin |
CN110951809A (en) * | 2019-09-04 | 2020-04-03 | 内蒙古立泰锐晟智能科技有限公司 | Process for preparing quinoa wheat polypeptide powder |
CN113372409A (en) * | 2021-06-08 | 2021-09-10 | 山东农业工程学院 | Method for extracting tenebrio molitor protein by ultrafine grinding-ultrasonic wave-microwave coupling |
Also Published As
Publication number | Publication date |
---|---|
CN107435060B (en) | 2021-02-09 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN105639014B (en) | A kind of polypeptide beverage and preparation method thereof | |
CN104489801A (en) | Preparation method of kelp health-care drink | |
CN107198252B (en) | Silkworm pupa protein, compound protein thereof and preparation method thereof | |
CN107435060A (en) | A kind of preparation method of longan nuclear protein polypeptide | |
CN104877876A (en) | Mulberry black rice wine and making method thereof | |
CN103642632A (en) | Preparation method of masa parasdisiac fruit wine | |
CN106616939A (en) | Stropharia rugoso-annulate bean flour and preparation method | |
CN104304480A (en) | Fast dissolving ginkgo nut milk tea and preparation method thereof | |
CN105294868A (en) | Extraction method for mushroom polysaccharide and preparation method for double-mushroom soup-stock essence | |
CN102860361A (en) | Processing method of low-purine soybean milk | |
CN104814439A (en) | Egg white mini-peptide antihypertensive nutrition powder and preparation method thereof | |
CN111670956B (en) | Mulberry leaf rice bean curd and preparation method thereof | |
CN113349356A (en) | Iceland red-pole ginseng intestine egg nutritional jelly and preparation method thereof | |
KR100503100B1 (en) | Process for low molecular weight peptide preparation from rice bran. | |
CN104232465A (en) | Production method of oyster mushroom rice vinegar | |
KR101186599B1 (en) | Method for Preparing Functional Beverage make use of Codonopsis lanceolata | |
CN105154308B (en) | The preparation technology of flue fruit vinegar | |
CN107647412A (en) | A kind of preparation method of longan nuclear protein polypeptide chewable tablets | |
CN107446753B (en) | Mulberry wine and preparation method thereof | |
CN106889624A (en) | A kind of preparation method of soya bean kind severe edema due to hypofunction of the spleen soluble dietary fiber | |
CN106819778A (en) | A kind of preparation method of water-soluble dietary fiber of corn peels | |
CN104232402A (en) | Preparation method of banana fruit wine | |
CN104178409A (en) | Method for preparing banana fruit vinegar | |
CN109363022A (en) | A kind of preparation method of Phyllanthus embical fruit sprouted unpolished rice vegetable protein dew | |
CN109123357A (en) | A kind of cucumber carrot glutinous rice cake and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |