CN104758203A - Macromolecular active aloe juice preparation method - Google Patents
Macromolecular active aloe juice preparation method Download PDFInfo
- Publication number
- CN104758203A CN104758203A CN201510103907.5A CN201510103907A CN104758203A CN 104758203 A CN104758203 A CN 104758203A CN 201510103907 A CN201510103907 A CN 201510103907A CN 104758203 A CN104758203 A CN 104758203A
- Authority
- CN
- China
- Prior art keywords
- aloe
- aloe juice
- large molecule
- molecule active
- juice
- 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
Landscapes
- Non-Alcoholic Beverages (AREA)
- Preparation Of Fruits And Vegetables (AREA)
Abstract
The invention relates to a macromolecular active aloe juice preparation method and belongs to the technical field of plant processing. The method includes following steps: (1) crushing and sterilizing aloe raw material to obtain aloe raw pulp; (2) purifying and centrifuging the aloe raw pulp to obtain aloe raw liquid; (3) performing ionic exchange adsorption to remove anthraquinone; and (4) finally performing sterilization to obtain macromolecular active aloe juice. The method is easy to operate and control and is good in anthraquinone removal effect. The macromolecular active aloe juice is less than 0.1 mg/kg in the content of aloin. The method allows employed resin to be recyclable, thereby reducing environmental pollution and production cost. Meanwhile, because the ionic exchange resin has specificity and is short in contact time, polysaccharides and functional components in the macromolecular active aloe juice are not loss. The method is excellent in social benefit and economical benefit.
Description
Technical field
The invention belongs to plant processing technique field, be specifically related to a kind of manufacture method of Large molecule active Aloe juice.
Background technology
Aloe is the evergreen herbage of Liliaceae, Aloe, originates in Mediterranean and Africa, american torrid zone is regional, also has distribution in Yunnan Province of China.Aloe is a kind of ancient, traditional conventional Chinese medicine, no matter in traditional medicine or modern medicine, has all affirmed the medical value of Aloe, and this has clear and definite record in China's medical book in one's early years and modern drug encyclopedia.Aloe has larger application in fields such as cosmetics, food, health product in recent years.Though China not as good as developed country, there has also been rapid progress in recent years, especially in aloe food and health product, compares extensive and deep research in the further investigation of Aloe, application and industrialization development.Along with the further exploitation of aloe food, aloe health product and Aloe cosmetics, particularly in the application of medicine field, there is higher requirement to the quality of aloe products, particularly without the aloe product that any degraded (enzymolysis) process, macromolecular polysaccharide fully retain, had very high demand.
Aloe is herbaceos perennial, containing a large amount of Anthraquinones and pectic substance in fresh aloe blade.Aloe anthraquinones class material has irritated effect to remove to skin, and the existence of pectin can make product instability (occurring layering and precipitation).Traditional method removing pectin adds enzyme preparation, makes pectin degrading, filters and remove.In interpolation enzyme preparation degrades process, the macromolecular polysaccharide in Aloe also can be degraded, and becomes micromolecular polysaccharide.The existence of pectin also add removing of anthraquinone, makes reservation Aloe macromolecular polysaccharide, and containing Aloe anthraquinones, the technical barrier not becoming production and processing containing the aloe product of aloe fibre.
Summary of the invention
For solving the degraded of aloe product macromolecular polysaccharide, removing the problems such as anthraquinone, the invention provides a kind of manufacture method of Large molecule active Aloe juice, substantially increase activity and the safety of aloe products, make Large molecule active aloe products can be used for food, cosmetics, improve the competitiveness of product in market.
The present invention is realized by following technical proposal:
A manufacture method for Large molecule active Aloe juice, comprises the steps:
A, by aloe leaf through cleaning, peeling, pasteurization after pulverizing, then is cooled to less than 30 DEG C, obtained Aloe oleo stock;
B, by steps A gained Aloe oleo stock successively through refining and centrifugal, get centrifugal after clear liquid, the mass percentage namely obtaining soluble solid is the aloe stoste of 0.75 ~ 2.0%;
C, be aloe Yuan Ye ︰ macroporous anion exchange resin=5 ~ 10 ︰ 1 by volume, by step B gained aloe stoste by macroporous anion exchange resin column, control 20 ~ 30min time of contact, namely obtain the Aloe juice I removing anthraquinone;
D, be Aloe juice Ⅰ ︰ strong-acid cation-exchange resin=40 ~ 50 ︰ 1 by volume, step C gained Aloe juice I exchanged tree post by strong-acid cation, controls 20 ~ 30min time of contact, namely obtain the Large molecule active Aloe juice II that pH is 3.5 ~ 5.0;
E, step D gained Aloe juice II is carried out pasteurization, then be cooled to less than 25 DEG C, through sterile filling, namely obtain Large molecule active Aloe juice.
Further, the temperature of the pasteurization preferably described in steps A is 75 ~ 85 DEG C, and the time is 15 ~ 30s.
Further, refining preferably described in step B is that employing 120 ~ 300 object refiner carries out, and removes the fiber in Aloe oleo stock and gel.
Further, the macroporous anion exchange resin preferably described in step C is food industry adsorbent resin, is commercial technical grade product.
Further, the strong-acid cation-exchange resin preferably described in step D is food industry adsorbent resin, is commercial technical grade product.
Further, the temperature of the pasteurization preferably described in step e is 90 ~ 95 DEG C, and the time is 15 ~ 30s.
compared with prior art, its beneficial effect is in the present invention:
The present invention uses 120 ~ 300 order refiners and secondary ion exchange adsorption to complete the production of Large molecule active Aloe juice, ion exchange resin has very high regeneration capacity and excellent antifouling property, in ion exchange process, the H on the anthraquinone in Aloe juice, inorganic salt and resin
+, OH
-exchange, thus reach the object removing anthraquinone, inorganic salt.
In the Aloe juice produced by the inventive method, Aloe macromolecular polysaccharide is without degraded, obtains abundant reservation, and Aloe polysaccharide mean molecule quantity reaches 1,300,000; Anthraquinone (barbaloin) is lower than 0.1mg/kg simultaneously, and product safety, without fiber in product, can be widely used in cosmetics, food.
Method of the present invention easily manipulates, anthraquinone and inorganic salt removal effect good, the resin of use can recycle, reduce environmental pollution, reduce production cost; Meanwhile, because ion exchange resin possesses specificity, time of contact is short, and polysaccharide and functional component do not lose, and has good economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the process chart of the manufacture method of Large molecule active Aloe juice of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting scope of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by buying the conventional products obtained.
In the present invention, 120 ~ 300 object refiners are commercial conventional equipment, purchased from but be not limited to Juneng Machinery (China) Co., Ltd..
Embodiment 1
As shown in Figure 1, a kind of manufacture method of Large molecule active Aloe juice, comprises the steps:
A, by 20 tons of aloe leafs through cleaning, peeling, pasteurization 15s after pulverizing, the temperature of pasteurization is 75 DEG C, and then is cooled to less than 30 DEG C, obtained Aloe oleo stock 11.4 tons;
B, by steps A gained Aloe oleo stock successively through refining and centrifugal, get centrifugal after clear liquid, the mass percentage namely obtaining soluble solid is the aloe stoste 9.7 tons of 1%;
C, be aloe Yuan Ye ︰ macroporous anion exchange resin=5 ︰ 1 by volume, by step B gained aloe stoste by commercial food industry macroporous anion exchange resin column, control 20min time of contact, namely obtain the Aloe juice I that 9.5 tons are removed anthraquinones;
D, be Aloe juice Ⅰ ︰ strong-acid cation-exchange resin=40 ︰ 1 by volume, step C gained Aloe juice I is exchanged tree post by commercial food industry strong-acid cation, control 20min time of contact, namely obtain the Large molecule active Aloe juice II that 9.1 tons of pH are 3.55;
E, step D gained Aloe juice II is carried out pasteurization 15s, the temperature of pasteurization is 90 DEG C, and then is cooled to less than 25 DEG C, through sterile filling, namely obtains the Large molecule active Aloe juice of Aloe polysaccharide mean molecule quantity more than 1,300,000.
Its molecular weight and molecular weight distribution detect as shown in table 1.
Table 1 Large molecule active Aloe juice molecular weight and molecular weight distribution detect table
Embodiment 2
As shown in Figure 1, a kind of manufacture method of Large molecule active Aloe juice, comprises the steps:
A, by 40 tons of aloe leafs through cleaning, peeling, pasteurization 15s after pulverizing, the temperature of pasteurization is 80 DEG C, then is cooled to less than 30 DEG C, obtained Aloe oleo stock 23.1 tons;
B, by steps A gained Aloe oleo stock successively through refining and centrifugal, get centrifugal after clear liquid, the mass percentage namely obtaining soluble solid is the aloe stoste 19.7 tons of 1.25%;
C, be aloe Yuan Ye ︰ macroporous anion exchange resin=10 ︰ 1 by volume, by step B gained aloe stoste by commercial food industry macroporous anion exchange resin column, control 20min time of contact, namely obtain the Aloe juice I that 19.3 tons are removed anthraquinones;
D, be Aloe juice Ⅰ ︰ strong-acid cation-exchange resin=50 ︰ 1 by volume, step C gained Aloe juice I is exchanged tree post by commercial food industry strong-acid cation, control 20min time of contact, namely obtain the Large molecule active Aloe juice II that 18.2 tons of pH are 3.72;
E, step D gained Aloe juice II is carried out pasteurization 15s, the temperature of pasteurization is 90 DEG C, then is cooled to less than 25 DEG C, through sterile filling, namely obtains the Large molecule active Aloe juice of Aloe polysaccharide mean molecule quantity more than 1,300,000.
Its molecular weight and molecular weight distribution detect as shown in table 2.
Table 2 Large molecule active Aloe juice molecular weight and molecular weight distribution detect table
Embodiment 3
As shown in Figure 1, a kind of manufacture method of Large molecule active Aloe juice, comprises the steps:
A, by 10 tons of aloe leafs through cleaning, peeling, pasteurization 15s after pulverizing, the temperature of pasteurization is 75 DEG C, then is cooled to 30 DEG C, obtained Aloe oleo stock 5.6 tons;
B, by steps A gained Aloe oleo stock adopt 120 ~ 300 object refiners refine, then centrifugal, get centrifugal after clear liquid, the mass percentage namely obtaining soluble solid is the aloe stoste 4.75 tons of 0.75%;
C, be aloe Yuan Ye ︰ macroporous anion exchange resin=5 ︰ 1 by volume, by step B gained aloe stoste by commercial food industry macroporous anion exchange resin column, control 20min time of contact, namely obtain the Aloe juice I that 4.5 tons are removed anthraquinones;
D, be Aloe juice Ⅰ ︰ strong-acid cation-exchange resin=40 ︰ 1 by volume, step C gained Aloe juice I is exchanged tree post by commercial food industry strong-acid cation, control 20min time of contact, namely obtain the Large molecule active Aloe juice II that 4.3 tons of pH are 3.5;
E, step D gained Aloe juice II is carried out pasteurization 15s, the temperature of pasteurization is 90 DEG C, then is cooled to 20 DEG C, through sterile filling, namely obtains the Large molecule active Aloe juice of Aloe polysaccharide mean molecule quantity more than 1,300,000.
Its molecular weight and molecular weight distribution detect as shown in table 3.
Table 3 Large molecule active Aloe juice molecular weight and molecular weight distribution detect table
Embodiment 4
As shown in Figure 1, a kind of manufacture method of Large molecule active Aloe juice, comprises the steps:
A, by 30 tons of aloe leafs through cleaning, peeling, pasteurization 30s after pulverizing, the temperature of pasteurization is 85 DEG C, then is cooled to 25 DEG C, obtained Aloe oleo stock 17.2 tons;
B, by steps A gained Aloe oleo stock adopt 120 ~ 300 object refiners refine, then centrifugal, get centrifugal after clear liquid, the mass percentage namely obtaining soluble solid is the aloe stoste 14.5 tons of 2.0%;
C, be aloe Yuan Ye ︰ macroporous anion exchange resin=10 ︰ 1 by volume, by step B gained aloe stoste by commercial food industry macroporous anion exchange resin column, control 30min time of contact, namely obtain the Aloe juice I that 13.7 tons are removed anthraquinones;
D, be Aloe juice Ⅰ ︰ strong-acid cation-exchange resin=50 ︰ 1 by volume, step C gained Aloe juice I is exchanged tree post by commercial food industry strong-acid cation, control 30min time of contact, namely obtain the Large molecule active Aloe juice II that 13 tons of pH are 3.76;
E, step D gained Aloe juice II is carried out pasteurization 30s, the temperature of pasteurization is 95 DEG C, then is cooled to 25 DEG C, through sterile filling, namely obtains the Large molecule active Aloe juice of Aloe polysaccharide mean molecule quantity more than 1,300,000.
Its molecular weight and molecular weight distribution detect as shown in table 4.
Table 4 Large molecule active Aloe juice molecular weight and molecular weight distribution detect table
Embodiment 5
As shown in Figure 1, a kind of manufacture method of Large molecule active Aloe juice, comprises the steps:
A, by 50 tons of aloe leafs through cleaning, peeling, pasteurization 22s after pulverizing, the temperature of pasteurization is 78 DEG C, then is cooled to 23 DEG C, obtained Aloe oleo stock 29.6 tons;
B, by steps A gained Aloe oleo stock adopt 120 ~ 300 object refiners refine, then centrifugal, get centrifugal after clear liquid, the mass percentage namely obtaining soluble solid is the aloe stoste 25.5 tons of 1.5%;
C, be aloe Yuan Ye ︰ macroporous anion exchange resin=7 ︰ 1 by volume, by step B gained aloe stoste by commercial food industry macroporous anion exchange resin column, control 23min time of contact, namely obtain the Aloe juice I that 24 tons are removed anthraquinones;
D, be Aloe juice Ⅰ ︰ strong-acid cation-exchange resin=45 ︰ 1 by volume, step C gained Aloe juice I is exchanged tree post by commercial food industry strong-acid cation, control 28min time of contact, namely obtain the Large molecule active Aloe juice II that 23.1 tons of pH are 3.67;
E, step D gained Aloe juice II is carried out pasteurization 25s, the temperature of pasteurization is 93 DEG C, then is cooled to 22 DEG C, through sterile filling, namely obtains the Large molecule active Aloe juice of Aloe polysaccharide mean molecule quantity more than 1,300,000.
Its molecular weight and molecular weight distribution detect as shown in table 5.
Table 5 Large molecule active Aloe juice molecular weight and molecular weight distribution detect table
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and description just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (6)
1. a manufacture method for Large molecule active Aloe juice, is characterized in that, comprises the steps:
A, by aloe leaf through cleaning, peeling, pasteurization after pulverizing, then is cooled to less than 30 DEG C, obtained Aloe oleo stock;
B, by steps A gained Aloe oleo stock successively through refining and centrifugal, get centrifugal after clear liquid, the mass percentage namely obtaining soluble solid is the aloe stoste of 0.75 ~ 2.0%;
C, be aloe Yuan Ye ︰ macroporous anion exchange resin=5 ~ 10 ︰ 1 by volume, by step B gained aloe stoste by macroporous anion exchange resin column, control 20 ~ 30min time of contact, namely obtain the Aloe juice I removing anthraquinone;
D, be Aloe juice Ⅰ ︰ strong-acid cation-exchange resin=40 ~ 50 ︰ 1 by volume, step C gained Aloe juice I exchanged tree post by strong-acid cation, controls 20 ~ 30min time of contact, namely obtain the Large molecule active Aloe juice II that pH is 3.5 ~ 5.0;
E, step D gained Aloe juice II is carried out pasteurization, then be cooled to less than 25 DEG C, through sterile filling, namely obtain Large molecule active Aloe juice.
2. the manufacture method of Large molecule active Aloe juice according to claim 1, is characterized in that, the temperature of the pasteurization described in steps A is 75 ~ 85 DEG C, and the time is 15 ~ 30s.
3. the manufacture method of Large molecule active Aloe juice according to claim 1, is characterized in that, refining described in step B is that employing 120 ~ 300 object refiner carries out.
4. the manufacture method of Large molecule active Aloe juice according to claim 1, is characterized in that, the macroporous anion exchange resin described in step C is food industry adsorbent resin, is commercial technical grade product.
5. the manufacture method of Large molecule active Aloe juice according to claim 1, is characterized in that, the strong-acid cation-exchange resin described in step D is food industry adsorbent resin, is commercial technical grade product.
6. the manufacture method of Large molecule active Aloe juice according to claim 1, is characterized in that, the temperature of the pasteurization described in step e is 90 ~ 95 DEG C, and the time is 15 ~ 30s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510103907.5A CN104758203B (en) | 2015-03-10 | 2015-03-10 | A kind of production method of Large molecule active asparagus juice |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510103907.5A CN104758203B (en) | 2015-03-10 | 2015-03-10 | A kind of production method of Large molecule active asparagus juice |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104758203A true CN104758203A (en) | 2015-07-08 |
| CN104758203B CN104758203B (en) | 2018-08-31 |
Family
ID=53640542
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510103907.5A Active CN104758203B (en) | 2015-03-10 | 2015-03-10 | A kind of production method of Large molecule active asparagus juice |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104758203B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107320409A (en) * | 2017-07-03 | 2017-11-07 | 云南万绿生物股份有限公司 | The preparation method of new Aloe Vera Gel |
| CN108208534A (en) * | 2017-12-10 | 2018-06-29 | 云南万绿生物股份有限公司 | A kind of processing method for removing aloe smell |
| CN108771091A (en) * | 2018-06-07 | 2018-11-09 | 云南万绿生物股份有限公司 | A kind of defecation method of Large molecule active asparagus juice |
| CN109731062A (en) * | 2018-11-30 | 2019-05-10 | 云南万绿生物股份有限公司 | A kind of preparation method of Large molecule active aloe frozen-dried powder |
| CN114272190A (en) * | 2022-01-19 | 2022-04-05 | 郑州凯莉莱生物科技有限公司 | Composition containing aloe active compound and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101053622A (en) * | 2006-04-14 | 2007-10-17 | 云南元江万绿生物（集团）有限公司 | Method for preparing aloe frozen-dried powder containing macro molecular substance |
| CN102824287A (en) * | 2012-09-07 | 2012-12-19 | 云南万绿生物股份有限公司 | Method for removing calcium and magnesium in aloe gel juice |
| CN103739725A (en) * | 2013-10-11 | 2014-04-23 | 云南万绿生物股份有限公司 | Refining method of aloe polysaccharide having high content and high purity |
| CN103877302A (en) * | 2014-03-22 | 2014-06-25 | 云南万绿生物股份有限公司 | Method for removing arsenic in aloe |
-
2015
- 2015-03-10 CN CN201510103907.5A patent/CN104758203B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101053622A (en) * | 2006-04-14 | 2007-10-17 | 云南元江万绿生物（集团）有限公司 | Method for preparing aloe frozen-dried powder containing macro molecular substance |
| CN102824287A (en) * | 2012-09-07 | 2012-12-19 | 云南万绿生物股份有限公司 | Method for removing calcium and magnesium in aloe gel juice |
| CN103739725A (en) * | 2013-10-11 | 2014-04-23 | 云南万绿生物股份有限公司 | Refining method of aloe polysaccharide having high content and high purity |
| CN103877302A (en) * | 2014-03-22 | 2014-06-25 | 云南万绿生物股份有限公司 | Method for removing arsenic in aloe |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107320409A (en) * | 2017-07-03 | 2017-11-07 | 云南万绿生物股份有限公司 | The preparation method of new Aloe Vera Gel |
| CN108208534A (en) * | 2017-12-10 | 2018-06-29 | 云南万绿生物股份有限公司 | A kind of processing method for removing aloe smell |
| CN108771091A (en) * | 2018-06-07 | 2018-11-09 | 云南万绿生物股份有限公司 | A kind of defecation method of Large molecule active asparagus juice |
| CN109731062A (en) * | 2018-11-30 | 2019-05-10 | 云南万绿生物股份有限公司 | A kind of preparation method of Large molecule active aloe frozen-dried powder |
| CN114272190A (en) * | 2022-01-19 | 2022-04-05 | 郑州凯莉莱生物科技有限公司 | Composition containing aloe active compound and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104758203B (en) | 2018-08-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104758203A (en) | Macromolecular active aloe juice preparation method | |
| CN102824287B (en) | Method for removing calcium and magnesium in aloe gel juice | |
| CN104558238B (en) | Process for extracting sodium alginate | |
| CN103739725B (en) | The process for purification of high-load high-purity aloe polysaccharide | |
| Jayasinghe et al. | Effect of extraction methods on the yield and physiochemical properties of polysaccharides extracted from seaweed available in Sri Lanka | |
| CN103263514A (en) | Method for extracting flavones, low-molecule pectin and cellulose from orange peels in combined way | |
| Safdar et al. | Influence of different extraction techniques on recovery, purity, antioxidant activities, and microstructure of flaxseed gum | |
| CN103564600A (en) | Natural food preservative and preparation method thereof | |
| Majdoub et al. | Water retention capacity of polysaccharides from prickly pear nopals of Opuntia ficus indica and Opuntia litoralis: Physical–chemical approach | |
| CN106496355B (en) | A kind of preparation method of pectin | |
| CN112480278A (en) | Bletilla striata polysaccharide and extraction method thereof | |
| CN104693314B (en) | Processing method for 2000: 1 aloe gel dry powder | |
| CN106074241B (en) | A kind of preparation method of activity aloe water | |
| CN111000779A (en) | Preparation method of aloe vera gel juice with low conductivity | |
| CN105249088B (en) | A kind of preparation method of pineapple concentration juice | |
| CN102887962A (en) | Method for preparing green tea polysaccharide through separation and purification and application of polysaccharide | |
| CN104738746A (en) | Method for processing small molecular active aloe juice | |
| CN103266150A (en) | Method for preparing functional oligosaccharides by utilizing beet pulp | |
| CN112442136A (en) | Method for extracting functional components from tremella | |
| CN110283860A (en) | The Gracilaria tenuistipitata polysaccharide and its extracting method of ultrasonic wave assisted recombination enzymolysis and extraction | |
| CN104693315A (en) | Processing method for 1000: 1 aloe gel dry powder | |
| Ukiwe et al. | Extraction of pectin from pineapple (Ananas comosus) peel using inorganic/organic acids and aluminum chloride | |
| CN112210022B (en) | Preparation method of low-methoxyl hawthorn pectin | |
| CN109851687B (en) | Method for separating and preparing fucoidin and algin from kelp | |
| CN110755459A (en) | Extraction process of annona squamosa leaf polyphenol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |