CN102048026B - Preparation method of oil-tea camellia meal protein polypeptide as additive for functional feeds - Google Patents
Preparation method of oil-tea camellia meal protein polypeptide as additive for functional feeds Download PDFInfo
- Publication number
- CN102048026B CN102048026B CN2010105729221A CN201010572922A CN102048026B CN 102048026 B CN102048026 B CN 102048026B CN 2010105729221 A CN2010105729221 A CN 2010105729221A CN 201010572922 A CN201010572922 A CN 201010572922A CN 102048026 B CN102048026 B CN 102048026B
- Authority
- CN
- China
- Prior art keywords
- protein polypeptide
- oil tea
- oil
- preparation
- rice
- 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.)
- Expired - Fee Related
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/87—Re-use of by-products of food processing for fodder production
Abstract
The invention relates to a preparation method of an oil-tea camellia meal protein polypeptide as an additive for functional feeds, comprising the following steps of, firstly, crushing a oil-tea camellia cake; secondly, removing saponin; thirdly, adding compound enzyme to carry out hydrolysis; fourthly, inactivating enzyme at the temperature of 80-90 DEG C for 5-15min; fifthly, carrying out centrifugal separation, and collecting supernate; sixthly, regulating a pH value of the supernate to be neutral; seventhly, filtering with a microporous membrane; and eighthly, carrying out low-temperature vacuum drying with the vacuum degree lower than 0.098MPa at the temperature of 35-55 DEG C to obtain the oil-tea camellia meal protein polypeptide. In the invention, the prepared oil-tea camellia meal protein polypeptide has the relative molecular mass lower than 1000Da, belongs to small molecular peptides, is safe to eat without bitter taste and toxicity, has strong immuno-modulating activity, and can efficiently enhance the survival rate and the weight growth rate of raised animals. The method provided by the invention can comprehensively utilize the agriculture waste resources, change the wastes into valuable and be beneficial to environmental protection, and has the advantages of low production cost and remarkable economic and social benefits.
Description
Technical field
The present invention relates to the preparation method of a kind of feed, relate in particular to the preparation method of a kind of functional feed with additive oil tea cake protein polypeptide with functional additive.
Background technology
At present, the by product albumen after the processing of fish meal and animal is most widely used protein source in livestock and poultry and the aquatic feeds always.But the problem that has three aspects: the first because receive global to excessively capture, EI Nino phenomenon and environmental pollution etc. influence, the output of fish meal descends year by year, the supply of world's fish meal at present can not have been satisfied growing breed demand; The second, in order to take precautions against the invasion of the spongy virus of ox brain, animal derived feed such as digested tankage are prohibited in many countries and regions, bone meal, and animal proteins such as meat meal tankage, blood meal, plasma powder, feather meal, whey powder are used in animal and fowl fodder; The 3rd, China's animal proteinum raw material resources are shortage very, mostly dependence on import.The price of high-quality animal-based protein is constantly soaring, has badly influenced the profit level of China's aquaculture.Oil tea cake protein polypeptide is to be that raw material is through conjugated protein enzymic hydrolysis after drying gained with the oil tea dregs of rice; This protein polypeptide has following advantage: it is rich in L-glutamic acid, l-arginine, leucine and aspartic acid (1); And amino acid is formed comprehensively, the fish-protein that its biological value (BV) and protein effect are used always near feed than (PER); (2) oil tea cake protein polypeptide is digested and assimilated by animal more easily, can improve the utilization ratio of feed, reduces production costs; (3) oil tea cake protein polypeptide has the excellent function activity; It has very strong anti-oxidant activity on the one hand; On the other hand; Tea seed protein polypeptide also has stronger immunoregulatory activity, can effectively improve by the resistance against diseases of feeding animals, reduce the use of medicine, thereby improve greatly by the security of feeding animals meat.Therefore oil tea cake protein polypeptide is a kind of fodder additives that is suitable as very much high economic worth animal, can add in the feed such as South America prawn, tilapia etc., as the conventional proteic senior substitute of feed.
Preparing at present oil meal protein polypeptide method commonly used is " extract albumen with alkali extraction and acid precipitation earlier and use the protease hydrolysis method again " or " grouts are directly used the microbial inoculant fermentation method that produces proteolytic enzyme "; The deadly defect of these methods has three: the protein denaturation that extract (1) is serious; Poorly water-soluble causes the efficient of follow-up protease hydrolyzed low; (2) environmental pollution is serious, and after the alkali extraction and acid precipitation method was extracted albumen, waste liquid is hard to manage, and was big to environmental influence; (3) grouts are directly used the microbial inoculant fermentation method that produces proteolytic enzyme, this method is because the protease activity that obtains is not strong, and hydrolysis ability is limited, and degree of hydrolysis is wayward, and fermentation time is long, and production efficiency is low.
Summary of the invention
The objective of the invention is to overcome the above-mentioned defective that existing protein polypeptide preparation method exists, provide a kind of protein denaturation few, water-soluble good, production efficiency is high, and the few functional feed of environmental pollution is with the preparation method of additive oil tea cake protein polypeptide.
The objective of the invention is to realize that through following technical scheme it may further comprise the steps:
(1) grouts of tea seed after oil expression is pulverized with kibbler, crossed 100 mesh sieves;
(2) use water extract method,, carry out tea saponin and separate according to solid masses and the ratio of liquid volume ratio for 1:7 ~ 13 (preferred 1:8 ~ 12); Extraction temperature is 65 ~ 85 ℃ (preferred 70 ~ 80 ℃); Extraction time is 6 ~ 10 h (preferred 7 ~ 9 h), and vat liquor pH value is 7.0, and lixiviate is centrifugal after accomplishing; Vat liquor is separated with the tea dregs of rice, obtain removing the oil tea dregs of rice of tea saponin;
(3) according to solid masses and the ratio of liquid volume ratio for 1:7 ~ 13 (preferred 1:8 ~ 12); To take off in the saponin oil tea dregs of rice adding clear water and soak 1 ~ 3 h (preferred 2 h); Regulate pH value to 8.0; Adding is the compound protease that 2 ~ 4:1 (preferred 3:1) forms by Sumizyme MP and flavor protease by mass ratio; The prozyme consumption places 45 ~ 55 ℃ of temperature (preferred 50 ℃) shaking bath hydrolysis 12 ~ 16 h (preferred 13 ~ 14 h) for removing 1 ~ 3 wt% (preferred 1.5 ~ 2.5 wt%) of the contained protein content of the oil tea dregs of rice (measuring with nitrogen determination) of tea saponin;
(4) after hydrolysis is accomplished, hydrolyzate is heated to 80 ~ 90 ℃ (preferred 85 ℃), keeps 5 ~ 15 min (preferred 8 ~ 12 min), make enzyme deactivation;
(5) spinning solid-liquid phase is collected supernatant;
(6) supernatant pH value is adjusted to neutrality;
(7) using the aperture is that the microporous membrane (optimization polypropylene macromolecular ultrafine fibrous membrane) of 0.1 ~ 1 μ m filters, and removes macromole;
(8) place vacuum tightness to be lower than 0.098 MPa, 35 ~ 55 ℃ of (preferred 40 ℃) low-temperature vacuum dryings, obtaining relative molecular mass is the oil tea cake protein polypeptide below 1000 Da.
Advantage of the present invention is that production cost is low, and the product that uses the inventive method to obtain is used for culturing, and animal surviving rate, rate of body weight gain significantly improve, and immunizing power obviously strengthens, and culture efficiency is obvious; Have no side effect; Can make the agricultural wastes resource obtain comprehensive utilization, turn waste into wealth, help environmental protection, economic and social benefit is remarkable.
Embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1
(1) grouts of tea seed after oil expression is pulverized with kibbler, crossed 100 mesh sieves;
(2) use water extract method, than being the ratio of 1:8, carrying out tea saponin and separate according to solid masses and liquid volume; Extraction temperature is 70 ℃, and extraction time is 9 h, and vat liquor pH value is 7.0; Lixiviate is centrifugal after accomplishing, and vat liquor is separated with the tea dregs of rice, obtains removing the oil tea dregs of rice of tea saponin;
(3) according to solid masses and liquid volume than being the ratio of 1:8; To take off the saponin oil tea dregs of rice and add immersion 2 h in the clear water; Regulate pH value to 8.0; Adding is the compound protease that 3:1 forms by flavor protease and Sumizyme MP by mass ratio, and the prozyme consumption places 50 ℃ of shaking bath hydrolysis 14 h of temperature for removing 1.5 wt% of the contained protein content of the oil tea dregs of rice (measuring with nitrogen determination) of tea saponin;
(4) after hydrolysis is accomplished, hydrolyzate is heated to 85 ℃, keeps 8 min, make enzyme deactivation;
(5) spinning solid-liquid phase is collected supernatant;
(6) hydrochloric acid with 0.5 mol/L is adjusted to neutrality with supernatant pH value;
(7) using the aperture is that the Vestolen PP 7052 macromolecular ultrafine fibrous membrane of 0.1 ~ 1 μ m filters, and removes macromole;
(8) place vacuum tightness to be lower than 0.098 MPa, 40 ℃ of low-temperature vacuum dryings obtain the oil tea cake protein polypeptide that relative molecular mass is lower than 1000 Da.
Embodiment 2
(1) grouts of tea seed after oil expression is pulverized with kibbler, crossed 100 mesh sieves;
(2) use water extract method, than being the ratio of 1:12, carrying out tea saponin and separate according to solid masses and liquid volume; Extraction temperature is 80 ℃, and extraction time is 7 h, and vat liquor pH value is 7.0; Lixiviate is centrifugal after accomplishing, and vat liquor is separated with the tea dregs of rice, obtains removing the oil tea dregs of rice of tea saponin;
(3) according to solid masses and liquid volume than being the ratio of 1:12; To take off the saponin oil tea dregs of rice and add immersion 2.0 h in the clear water; Regulate pH value to 8.0; Adding is the compound protease that 3:1 forms by flavor protease and Sumizyme MP by mass ratio, and the prozyme consumption places 50 ℃ of shaking bath hydrolysis 13 h of temperature for removing 2.5 wt% of the contained protein content of the oil tea dregs of rice (measuring with nitrogen determination) of tea saponin;
(4) after hydrolysis is accomplished, hydrolyzate is heated to 85 ℃, keeps 12 min, make enzyme deactivation;
(5) spinning solid-liquid phase is collected supernatant;
(6) hydrochloric acid with 0.5 mol/L is adjusted to neutrality with supernatant pH value;
(7) using the aperture is that the Vestolen PP 7052 macromolecular ultrafine fibrous membrane of 0.1 ~ 1 μ m filters, and removes macromole;
(8) place vacuum tightness to be lower than 0.098 MPa, 40 ℃ of low-temperature vacuum dryings obtain the oil tea cake protein polypeptide that relative molecular mass is lower than 1000 Da.
Embodiment 3
In every kilogram of feed, add the oil tea cake protein polypeptide of 500 mg embodiment, 1 preparation and feed 5 weeks of Penaeus vannamei, compare with basal feed group (not adding oil tea cake protein polypeptide), its surviving rate has improved 15.2%; Rate of body weight gain has improved 25.4%; (the serum lysozyme vigor has improved 49.1%, and the acid phosphatase enzyme activity has improved 63.7%, and alkaline phosphatase activity has improved 59.3% in the immunizing power enhancing; Superoxide dismutase activity has improved 61.5%; Mda content has reduced by 21.6%, and the vigor of said enzyme and MDA content all adopt Nanjing to build up the corresponding reagent box that bio-engineering research is produced, and measure with spectrophotometry).
Embodiment 4
In every kilogram of feed, add the oil tea cake protein polypeptide of 1000 mg embodiment, 1 preparation and feed 5 weeks of Penaeus vannamei, compare with basal feed group (not adding oil tea cake protein polypeptide), its surviving rate has improved 20.4%; Rate of body weight gain has improved 32.6%; (the serum lysozyme vigor has improved 56.8%, and the acid phosphatase enzyme activity has improved 75.9%, and alkaline phosphatase activity has improved 70.8% in the immunizing power enhancing; Superoxide dismutase activity has improved 76.2%; Mda content has reduced by 27.9%, and the vigor of said enzyme and MDA content all adopt Nanjing to build up the corresponding reagent box that bio-engineering research is produced, and measure with spectrophotometry).
Embodiment 5
In every kilogram of feed, add the oil tea cake protein polypeptide of 1500 mg embodiment, 2 preparations and feed 5 weeks of Penaeus vannamei, compare with basal feed group (not adding oil tea cake protein polypeptide), its surviving rate has improved 24.7%; Rate of body weight gain has improved 38.8%; (the serum lysozyme vigor has improved 60.3%, and the acid phosphatase enzyme activity has improved 82.1%, and alkaline phosphatase activity has improved 76.8% in the immunizing power enhancing; Superoxide dismutase activity has improved 83.4%; Mda content has reduced by 33.7%, and the vigor of said enzyme and MDA content all adopt Nanjing to build up the corresponding reagent box that bio-engineering research is produced, and measure with spectrophotometry).
Embodiment 6
In every kilogram of feed, add the oil tea cake protein polypeptide of 2000 mg embodiment, 2 preparations and feed 5 weeks of Penaeus vannamei, compare with basal feed group (not adding oil tea cake protein polypeptide), its surviving rate has improved 26.3%; Rate of body weight gain has improved 41.2%; (the serum lysozyme vigor has improved 63.1%, and the acid phosphatase enzyme activity has improved 84.9%, and alkaline phosphatase activity has improved 78.5% in the immunizing power enhancing; Superoxide dismutase activity has improved 85.1%; Mda content has reduced by 35.2%, and the vigor of said enzyme and MDA content all adopt Nanjing to build up the corresponding reagent box that bio-engineering research is produced, and measure with spectrophotometry).
Claims (6)
1. a functional feed is characterized in that may further comprise the steps with the preparation method of additive oil tea cake protein polypeptide:
(1) grouts of tea seed after oil expression is pulverized with kibbler, crossed 100 mesh sieves;
(2) use water extract method, than being the ratio of 1:7 ~ 13, carrying out tea saponin and separate according to solid masses and liquid volume; Extraction temperature is 65 ~ 85 ℃, and extraction time is 6 ~ 10 h, and vat liquor pH value is 7.0; Lixiviate is centrifugal after accomplishing, and vat liquor is separated with the tea dregs of rice, obtains removing the oil tea dregs of rice of tea saponin;
(3) according to solid masses and liquid volume than being the ratio of 1:7 ~ 13; To take off in the saponin oil tea dregs of rice adding clear water and soak 1 ~ 3 h; Regulate pH value to 8.0, adding by Sumizyme MP and flavor protease is the compound protease that 2 ~ 4:1 forms by mass ratio, places 45 ~ 55 ℃ of shaking bath hydrolysis 12 ~ 16 h of temperature; The prozyme consumption is for remove 1 ~ 3 wt% of the contained protein content of the oil tea dregs of rice of tea saponin, and the contained protein content of the oil tea dregs of rice that has removed tea saponin is measured with nitrogen determination;
(4) after hydrolysis is accomplished, hydrolyzate is heated to 80 ~ 90 ℃, keeps 5 ~ 15 min, make enzyme deactivation;
(5) spinning solid-liquid phase is collected supernatant;
(6) supernatant pH value is adjusted to neutrality;
(7) using the aperture is that the microporous membrane of 0.1 ~ 1 μ m filters, and removes macromole;
(8) place vacuum tightness to be lower than 0.098 MPa, 35 ~ 55 ℃ of low-temperature vacuum dryings obtain oil tea cake protein polypeptide.
2. functional feed according to claim 1 is with the preparation method of additive oil tea cake protein polypeptide; It is characterized in that the said water extract method of step (2); According to solid masses and liquid volume than being the ratio of 1:8 ~ 12; Carry out tea saponin and separate, extraction temperature is 70 ~ 80 ℃, and extraction time is 7 ~ 9 h.
3. functional feed according to claim 1 is with the preparation method of additive oil tea cake protein polypeptide; It is characterized in that step (3) said according to solid masses and liquid volume than being the ratio of 1:8 ~ 12; To take off the saponin oil tea dregs of rice and add immersion 2 h in the clear water; Adding is the compound protease that 3:1 forms by Sumizyme MP and flavor protease by mass ratio; The prozyme consumption places 50 ℃ of shaking bath hydrolysis 13 ~ 14 h of temperature for removing 1.5 ~ 2.5 wt% of the contained protein content of the oil tea dregs of rice of tea saponin.
4. functional feed according to claim 1 is with the preparation method of additive oil tea cake protein polypeptide, it is characterized in that the said hydrolysis of step (4) is accomplished after, hydrolyzate is heated to 85 ℃, keep 8 ~ 12 min, make enzyme deactivation.
5. functional feed according to claim 1 is with the preparation method of additive oil tea cake protein polypeptide, it is characterized in that the said use of step (7) aperture is that the Vestolen PP 7052 macromolecular ultrafine fibrous membrane of 0.1 ~ 1 μ m filters, and removes macromole.
6. functional feed according to claim 1 is characterized in that with the preparation method of additive oil tea cake protein polypeptide the said vacuum tightness that places of step (8) is lower than 0.098 MPa, and 40 ℃ of low-temperature vacuum dryings obtain oil tea cake protein polypeptide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105729221A CN102048026B (en) | 2010-12-06 | 2010-12-06 | Preparation method of oil-tea camellia meal protein polypeptide as additive for functional feeds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105729221A CN102048026B (en) | 2010-12-06 | 2010-12-06 | Preparation method of oil-tea camellia meal protein polypeptide as additive for functional feeds |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102048026A CN102048026A (en) | 2011-05-11 |
| CN102048026B true CN102048026B (en) | 2012-12-05 |
Family
ID=43953095
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105729221A Expired - Fee Related CN102048026B (en) | 2010-12-06 | 2010-12-06 | Preparation method of oil-tea camellia meal protein polypeptide as additive for functional feeds |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102048026B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103484517B (en) * | 2013-09-11 | 2016-03-02 | 邹远东 | A kind of camellia seed protein peptide and preparation method thereof and its application |
| CN104531814B (en) * | 2014-12-05 | 2017-11-14 | 中南林业科技大学 | A kind of preparation method of Extracted From Oil-tea-cake enzyme modification albumen |
| CN104450846B (en) * | 2014-12-05 | 2018-05-01 | 中南林业科技大学 | A kind of Extracted From Oil-tea-cake protein blood pressure-reducing peptide semi continuous preparation method |
| CN107259101A (en) * | 2017-02-13 | 2017-10-20 | 中南林业科技大学 | A kind of method of camellia seed meal ferment making feed |
| WO2019114159A1 (en) * | 2017-12-11 | 2019-06-20 | 盛蓓蓓 | Camellia oleifera meal polypeptide and polysaccharide as well as preparation method and application thereof, and camellia oleifera meal detoxification method |
| CN108060196B (en) * | 2017-12-11 | 2018-11-27 | 正大联合动物制药科技（江苏）有限公司 | A kind of Extracted From Oil-tea-cake polypeptide, preparation method and the effect for promoting weary feelings estrus of cow and fertilization |
| CN114686552A (en) * | 2022-04-02 | 2022-07-01 | 吉林农业大学 | Preparation method of camellia seed meal polypeptide zinc chelate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1439720A (en) * | 2003-01-30 | 2003-09-03 | 大连理工大学 | Soya protein oligopeptides production |
| CN101570773A (en) * | 2009-05-27 | 2009-11-04 | 中国农业科学院油料作物研究所 | Method for producing active polypeptide by microwave aid enzymolysis of oil meal protein |
-
2010
- 2010-12-06 CN CN2010105729221A patent/CN102048026B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1439720A (en) * | 2003-01-30 | 2003-09-03 | 大连理工大学 | Soya protein oligopeptides production |
| CN101570773A (en) * | 2009-05-27 | 2009-11-04 | 中国农业科学院油料作物研究所 | Method for producing active polypeptide by microwave aid enzymolysis of oil meal protein |
Non-Patent Citations (3)
| Title |
|---|
| 姚玉静等.复合蛋白酶水解豆粕制备呈味基料的研究.《现代食品科技》.2007,第23卷(第6期),8-10. * |
| 曾馥平等.脱毒油茶枯饼营养价值研究.《中国饲料》.1992,(第5期),28-29. * |
| 龚吉军等.茶籽多肽的制备及体外抗氧化活性研究.《农业与技术》.2006,第26卷(第6期),74-77. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102048026A (en) | 2011-05-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104892037B (en) | A kind of take fish as the method for the water-soluble fish-protein organic fertilizer of raw material production | |
| CN102048026B (en) | Preparation method of oil-tea camellia meal protein polypeptide as additive for functional feeds | |
| CN102488180A (en) | Method for preparing natural mutton flavour by utilizing sheep bone | |
| CN108477619A (en) | A kind of preparation method of compound amino acid chelate calcium | |
| CN102154422B (en) | Method for extracting functional small peptides from low-value sea fish | |
| CN100496277C (en) | Mantis shrimp protein pulp and its producing process | |
| CN105624249A (en) | Preparation method of aquatic protein and plant protein compound active peptide | |
| CN101632412A (en) | Compound aquatic product attractant and processing method thereof | |
| CN106962590A (en) | A kind of method for preparing edible fungus protein powder | |
| CN1555720A (en) | Poly peptide protein feed and its processing method | |
| CN107455441A (en) | A kind of method for digesting silver carp by-product production minced fillet antifreeze | |
| CN101984854B (en) | Method for producing purely natural monosodium glutamate by using low-value marine fishes | |
| CN103045705A (en) | Method for producing protein peptide composed of fish protein peptide and soybean peptide | |
| CN104431360A (en) | Bellamya paste and production process thereof | |
| CN1260183C (en) | Preparation method of fish protein biological peptide fertilizer | |
| CN1161303C (en) | Process for preparing nourishing agent of plant | |
| CN1788598A (en) | Protein feed stuff and processing method thereof | |
| KR20170079910A (en) | Feed additives for abalone | |
| CN103168915A (en) | Copepoda peptide paste and production process thereof | |
| WO2011108810A2 (en) | Amino acid liquid fertilizer using marine waste, and preparation method thereof | |
| CN105154507B (en) | A kind of feed grade ocean fish oligopeptide powder and its application | |
| US20220009850A1 (en) | Production of organic fertilizer from aquatic organisms | |
| CN107176865A (en) | The sweetened liquid fertilizer method of preparation and use of marine alga earthworm hydrolyzate efficient bio-active | |
| CN105995653A (en) | Method for preparing artemia-cysts-shell hydrolyzing liquid | |
| CN109097428B (en) | Preparation method of fish protein peptide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20121205 Termination date: 20151206 |
|
| EXPY | Termination of patent right or utility model |