CN105232494A - Celecoxib capsules and production technology thereof - Google Patents
Celecoxib capsules and production technology thereof Download PDFInfo
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- CN105232494A CN105232494A CN201510770019.9A CN201510770019A CN105232494A CN 105232494 A CN105232494 A CN 105232494A CN 201510770019 A CN201510770019 A CN 201510770019A CN 105232494 A CN105232494 A CN 105232494A
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Abstract
The invention discloses celecoxib capsules. The celecoxib capsules are prepared from celecoxib, lactose monohydrate, povidone, crosslinking sodium carboxymethylcellulose, lauryl sodium sulfate and magnesium stearate. The invention also discloses a production technology of the celecoxib capsules. The production technology comprises the steps of material distribution, preparation of a granulation solution, premixing, granulation, wet size stabilization, drying, dry size stabilization, final mixing, granule discharging, capsule filling and packaging. The celecoxib capsules and the production technology thereof have the advantages that formulation raw materials are low in cost, and the technology is simple; the dissolution rate of celecoxib is high, and celecoxib can be easily absorbed by the human body.
Description
Technical field
The present invention relates to chemical medicine field, particularly relate to a kind of Celebret and production technology thereof.
Background technology
Celecoxib (Celecoxib), i.e. 4-[5-(4-tolyl)-3-(trifluoromethyl)-1 hydrogen-1-pyrazol-1-yl] benzsulfamide, first Selective COX-2 inhibitor, also be the maximum non_steroidal anti_inflammatory drug of current global recipe quantity, not only there is remarkable analgesia effect, significantly can alleviate joint tenderness, pain and arthroncus, and there is superior gastrointestinal safety, according to the SUCCESS research report that " JAMA " is delivered for 2006, relate in the comparative study of 39 national 13274 routine patients at one, the probability that symptomatic ulcer and ulcer complication occur celecoxib group patient is lower by 87.5% than the patient of traditional non_steroidal anti_inflammatory drug group.Because celecoxib chance light is perishable, there is hygroscopicity; Prove through test, all easily there is variable color and go bad in Celebret and raw material medicine solution, reduce the drug effect of Celebret under illumination and aerobic conditions.
But celecoxib dissolubility is extremely low, at 25 DEG C, in water, dissolubility is about 0.007mg/ml, and in conventional dissolution medium, stripping is slow, and its quality standard adopts the sodium radio-phosphate,P-32 solution of pH12.As everyone knows, the stripping of medicine is the prerequisite playing therapeutical effect, how to promote celecoxib stripping fast and completely, is the problem that those skilled in the art need to put forth effort to solve.Celecoxib is a kind of insoluble drug, is insoluble to unusually in water-bearing media.And for poorly water-soluble the normal oral solid preparation of high osmosis medicine, because stripping is often the speed limit process of absorption process, thus dissolution be affect insoluble drug absorption thus affect the most key characteristic of curative effect of medication.Research simultaneously shows that the dissolution of medicine and chemical factors, prescription and the production technology such as crystal formation, granularity of medicine have close relationship.The algoscopy registering the dissolution defining Celebret in quality standard JX20000001 in the import of Celebret as with 0.04M trisodium phosphate solution (regulating pH12.0 ± 0.1 with phosphoric acid or the sodium hydroxide test solution) 1000ml containing 1% sodium lauryl sulphate for solvent, rotating speed is 50 turns per minute, measures the dissolution of its every capsules for being not less than 75% through 45 minutes.
The wet granulation that the many employings of capsule are traditional, production process is more, mainly through supplementary material mixing, prepare soft material, granulation, drying, arrangement, total mixed, filling, polishing, bubble-cap, operation is relatively loaded down with trivial details, consuming time longer.Make celecoxib in process of production variable color deterioration happen occasionally, it is large that medicine quality homogeneity controls difficulty, and between batch, quality fluctuation is remarkable, is unfavorable for patient safety medication.
Chinese patent CN103989657A discloses a kind of capsule containing celecoxib, containing 40wt%-70wt% celecoxib, 22wt%-50wt% water-soluble filler, 0.5wt%-25wt% low-substituted hydroxypropyl cellulose, 0.5wt%-10wt% sodium lauryl sulphate, the production technology that this invention is not special, for capsule dissolution in vivo without any improvement, affect absorption of human body.Chinese patent CN104382877A discloses a kind of Celebret, is grouped into by the following one-tenth of weight part ratio, celecoxib 30-100 part, starch 25-50 part, lubricant 5-10 part, also discloses a kind of preparation method, takes celecoxib and starch by formula proportion, dry granulation, after adding the lubricant mixing of formula proportion, filling, polishing, bubble-cap, obtain Celebret, but this method cost of manufacture is higher, stripping is unstable.Chinese patent CN104721169A discloses kind Celebret and preparation method thereof, comprise active component celecoxib and organic acid, calcium carbonate or the pharmaceutic adjuvant such as sodium bicarbonate, lactose, but comparatively significantly do not improve, for this key point of dissolution without any improvement on process means yet.
Summary of the invention
In order to solve celecoxib medicine in use, dissolution is lower, is difficult to the problem be absorbed by the body, and we have proposed a kind of Celebret and production technology thereof, adopts the present invention to reach absorption efficiency high, the object that dissolution is high.
The present invention is achieved by the following technical solutions:
For achieving the above object, the invention provides a kind of Celebret, comprise the raw material of following mass percent:
Celecoxib: 74.07%;
Lactose monohydrate: 18.43%; Lactose monohydrate, as filler and correctives, can also prevent crystallization, bonding, and the form quality for capsule has control potentiation;
Polyvidone: 2.5%; Polyvidone a kind of water misciblely has efficient fusible synthetic polymer, mainly as the binding agent of solid preparation wet granulation, its special performance makes to become and important excipient in the application of various oral liquid, suspensoid and locality drug development.
Cross-linking sodium carboxymethyl cellulose: 1%; Crosslinked cross-linking sodium carboxymethyl cellulose is the Powdered natural product obtained through crosslinked, pulverizing by the cellulose of pure natural, and sophistication is good, and the disintegrate for capsule has good facilitation;
Sodium lauryl sulphate: 3%; Be a kind of white or faint yellow micro-sticky thing, be industrially usually used in detergent and textile industry.Belong to anion surfactant.Soluble in water, compatibility is good again with anion, nonionic, there is good emulsifying, foaming, infiltration, decontamination and dispersive property, be widely used in toothpaste, shampoo, hair cream, shampoo, detergent, liquid washed, cosmetics and the plastics demoulding, the industries such as lubrication and pharmacy, papermaking, building materials, chemical industry.
Magnesium stearate: 1%.Magnesium stearate is hydrophobic lubricant, and easy and granule mixes, unilateral smooth and beautiful appearance after tabletting.
Invention also provides a kind of production technology of Celebret, step is as follows:
(1) sub-material:
Take each material according to batch prescription respectively between weighing, insert in PE bag, and put into stainless steel cask, concentrate and place.With batch prescription for standard, a collection of 8.10kg, its Raw celecoxib 5.265-6.885kg, operative norm is with reference to " USP current edition ", filler lactose monohydrate 0.92-2.025kg, operative norm is with reference to " 2010 editions Chinese Pharmacopoeias ", binding agent polyvidone 0.081-0.405kg, operative norm is with reference to " 2010 editions Chinese Pharmacopoeias ", disintegrating agent cross-linking sodium carboxymethyl cellulose 0.041-0.162kg, operative norm is with reference to " 2010 editions Chinese Pharmacopoeias ", wetting agent sodium lauryl sulphate 0.081-0.405kg, operative norm is with reference to " 2010 editions Chinese Pharmacopoeias ", magnesium stearate lubricant 0.041-0.162kg, operative norm is with reference to " 2010 editions Chinese Pharmacopoeias ".
(2) preparation of granulation solution:
In rustless steel container, add deionized water, stirring to forming whirlpool, slowly adding sodium lauryl sulphate, continue stirring more than 15 minutes with the speed that can form whirlpool, dispersion is until all dissolve, and solution is limpid.
(3) premix:
Successively celecoxib, cross-linked carboxymethyl cellulose are received, polyvidone, lactose monohydrate shift in high shear granulator, use following parameters mixing:
Mixing speed: 150rpm;
Cutting knife speed: 2000rpm;
Incorporation time: 300s.
(4) granulate:
Start after premix, to mixed material spray granulation solution, to use following parameters to granulate:
Nozzle model: 6501;
Nozzle diameter: 1mm;
Nozzle location: distance 3.5 centimetres, top;
Peristaltic pump rotating speed: 300rpm;
Mixing speed: 150rpm;
Granulation speed: 2000rpm;
Granulation time: 360s.
(5) wet granulate:
Transfer in fluid bed by wet granular by pelletizing machine, parameter is as follows:
Mixing speed: 30rpm;
Mesh size: 2.5 × 3.5mm;
Granulate speed: 300rpm.
(6) dry:
Inlet temperature: 65 DEG C ± 5 DEG C;
Tremble a bag time: 16 seconds;
Tremble a bag interval: 30 seconds;
At fluidized dryer inner drying granule until temperature of charge reaches 35 DEG C, detect LOD with fast tester for water content at 105 DEG C.
(7) dry granulate:
After dried granule crosses 24 eye mesh screens, the above granule of 24 eye mesh screen is weighed.
(8) mixed eventually:
Loaded in mixer by granule after granulate, magnesium stearate is crossed 30 mesh sieves and is entered mixer and mix by following parameters:
Mixing velocity: 15rpm;
Incorporation time: 10 minutes.
(9) granule is unloaded:
Granule after lubrication is installed in bucket or mixer, fastens lid and granule left in hermetic container is medium is ready to use in fill capsule, weigh and calculated yield.
(10) capsule fill:
With capsule and corresponding mould according to theoretical weight fill, directly loaded in PE bag by capsule good for fill, capsule adopts No. 2 gelatine capsules.
(11) pack:
Use following parameters capsule is loaded aluminum-plastic packaged in:
Upper heating-up temperature: 120 DEG C;
Lower heating-up temperature: 120 DEG C;
Heat-sealing temperature: 180 DEG C;
Compressed air pressure: 0.8MPa.
Preferably, in above-mentioned steps (4) during spray granulation solution, a small amount of pure water can be added as required.
Compared with prior art, beneficial effect of the present invention is:
1, formula material is with low cost, and technique is simple;
2, celecoxib dissolution is higher, is easily absorbed by the body.
Detailed description of the invention
Below in conjunction with embodiment, further illustrate content of the present invention.Should be appreciated that enforcement of the present invention is not limited to the following examples, any pro forma accommodation make the present invention or change all fall into scope; And the method in following embodiment, if no special instructions, be the conventional method of this area.
Embodiment 1:
A kind of Celebret, comprises the raw material of following mass percent: celecoxib: 65.43%; Lactose monohydrate: 25.31%; Polyvidone: 4.07%; Cross-linking sodium carboxymethyl cellulose: 0.56%; Sodium lauryl sulphate: 4.07%; Magnesium stearate: 0.56%.In batches (8.10kg) to produce prescription as follows: celecoxib 5.3kg, lactose monohydrate 2.05kg, polyvidone 0.33kg, cross-linking sodium carboxymethyl cellulose 0.045kg, sodium lauryl sulphate 0.33kg, magnesium stearate 0.045kg.
Production stage is as follows:
(1) sub-material: take each material according to batch prescription respectively between weighing, insert in PE bag, and put into stainless steel cask, concentrates and places.
(2) preparation of granulation solution: add deionized water in rustless steel container, stirring to forming whirlpool, slowly adding sodium lauryl sulphate, and continue stirring more than 15 minutes with the speed that can form whirlpool, dispersion is until all dissolve, and solution is limpid.
(3) premix: successively celecoxib, cross-linked carboxymethyl cellulose are received, polyvidone, lactose monohydrate shift in high shear granulator, use following parameters mixing: mixing speed: 150rpm; Cutting knife speed: 2000rpm; Incorporation time: 300s.
(4) granulate: start after premix, to mixed material spray granulation solution, to use following parameters to granulate:
Nozzle model: 6501; Nozzle diameter: 1mm; Nozzle location: distance 3.5 centimetres, top; Peristaltic pump rotating speed: 300rpm; Mixing speed: 150rpm; Granulation speed: 2000rpm; Granulation time: 360s.
(5) wet granulate: transfer in fluid bed by wet granular by pelletizing machine, parameter is as follows:
Mixing speed: 30rpm; Mesh size: 2.5 × 3.5mm; Granulate speed: 300rpm.
(6) dry: inlet temperature: 65 DEG C ± 5 DEG C; Tremble a bag time: 16 seconds; Tremble a bag interval: 30 seconds; At fluidized dryer inner drying granule until temperature of charge reaches 35 DEG C, detect LOD with fast tester for water content at 105 DEG C.
(7) dry granulate: after dried granule crosses 24 eye mesh screens, weighs the above granule of 24 eye mesh screen.
(8) mixed eventually: loaded in mixer by the granule after granulate, magnesium stearate is crossed 30 mesh sieves and entered mixer and mix by following parameters: mixing velocity: 15rpm; Incorporation time: 10 minutes.
(9) unload granule: installed in bucket or mixer by the granule after lubrication, fasten lid and granule left in hermetic container is medium is ready to use in fill capsule, weigh and calculated yield.
(10) capsule fill: use capsule and corresponding mould according to theoretical weight fill, directly capsule good for fill is loaded in PE bag.
(11) pack: use following parameters capsule is loaded aluminum-plastic packaged in: upper heating-up temperature: 120 DEG C; Lower heating-up temperature: 120 DEG C; Heat-sealing temperature: 180 DEG C; Compressed air pressure: 0.8MPa.
(12) detect: Celebret embodiment prepared gets 20-40 grain at random respectively according to the method for " 2010 editions Chinese Pharmacopoeias " two annex × C second methods, measure it containing the dissolution in 0.04M trisodium phosphate solution (regulating pH12.0 ± 0.1 with phosphoric acid or the sodium hydroxide test solution) 1000mL of 1% sodium lauryl sulphate, its result is as shown in table 1.
Embodiment 2:
A kind of Celebret, comprises the raw material of following mass percent: celecoxib: 74.07%; Lactose monohydrate: 18.43%; Polyvidone: 2.5%; Cross-linking sodium carboxymethyl cellulose: 1%; Sodium lauryl sulphate: 3%; Magnesium stearate: 1%.In batches (8.10kg) to produce prescription as follows: celecoxib 6.00kg, lactose monohydrate 1.50kg, polyvidone 0.20kg, cross-linking sodium carboxymethyl cellulose 0.08kg, sodium lauryl sulphate 0.24kg, magnesium stearate 0.08kg.
Production stage is substantially the same manner as Example 1, and detecting step is also substantially the same manner as Example 1.
Embodiment 3:
A kind of Celebret, comprises the raw material of following mass percent: celecoxib: 84.57%; Lactose monohydrate: 12.22%; Polyvidone: 1.05%; Cross-linking sodium carboxymethyl cellulose: 0.56%; Sodium lauryl sulphate: 1.05%; Magnesium stearate: 0.56%.In batches (8.10kg) to produce prescription as follows: celecoxib 6.85kg, lactose monohydrate 0.99kg, polyvidone 0.085kg, cross-linking sodium carboxymethyl cellulose 0.045kg, sodium lauryl sulphate 0.085kg, magnesium stearate 0.045kg.
Production stage is substantially the same manner as Example 1, and detecting step is also substantially the same manner as Example 1.
Comparative example 1:
Formula is substantially the same manner as Example 1, and production stage uses conventional wet to granulate, and detecting step is also substantially the same manner as Example 1.
Comparative example 2:
Formula is substantially the same manner as Example 2, and production stage uses conventional wet to granulate, and detecting step is also substantially the same manner as Example 1.
Comparative example 3:
Formula is substantially the same manner as Example 3, and production stage uses conventional wet to granulate, and detecting step is also substantially the same manner as Example 1.
Comparative example 4:
Commercial common Celebret, detecting step is also substantially the same manner as Example 1.
Table 1:
As seen from the above table, through the Celebret that the present invention makes, on dissolution, comparatively conventional wet lay granulation Celebret has greatly improved, and particularly more than high-dissolution (92%) has accounted for the nearly ratio of half, has improve much for absorbing of medicine.And according to our company since in July, 2011, Celebret production line put into production, comparatively wet granulation produces Celebret, energy-conservation 28%, production efficiency improves 59%.
Claims (3)
1. a Celebret, is characterized in that, described capsule comprises the raw material of following mass percent:
Celecoxib: 65-85%;
Lactose monohydrate: 12-25%;
Polyvidone: 1-5%;
Cross-linking sodium carboxymethyl cellulose: 0.5-2%;
Sodium lauryl sulphate: 1-5%;
Magnesium stearate: 0.5-2%.
2. a production technology for Celebret, is characterized in that, step is as follows:
(1) sub-material:
Take each material according to batch prescription respectively between weighing, insert in PE bag, and put into stainless steel cask, concentrate and place;
(2) preparation of granulation solution:
In rustless steel container, add deionized water, stirring to forming whirlpool, slowly adding sodium lauryl sulphate, continue stirring more than 15 minutes with the speed that can form whirlpool, dispersion is until all dissolve, and solution is limpid;
(3) premix:
Successively celecoxib, cross-linked carboxymethyl cellulose are received, polyvidone, lactose monohydrate shift in high shear granulator, use following parameters mixing:
Mixing speed: 150rpm;
Cutting knife speed: 2000rpm;
Incorporation time: 300s;
(4) granulate:
Start after premix, to mixed material spray granulation solution, to use following parameters to granulate:
Nozzle model: 6501;
Nozzle diameter: 1mm;
Nozzle location: distance 3.5 centimetres, top;
Peristaltic pump rotating speed: 300rpm;
Mixing speed: 150rpm;
Granulation speed: 2000rpm;
Granulation time: 360s;
(5) wet granulate:
Transfer in fluid bed by wet granular by pelletizing machine, parameter is as follows:
Mixing speed: 30rpm;
Mesh size: 2.5 × 3.5mm;
Granulate speed: 300rpm;
(6) dry:
Inlet temperature: 65 DEG C ± 5 DEG C;
Tremble a bag time: 16 seconds;
Tremble a bag interval: 30 seconds;
At fluidized dryer inner drying granule until temperature of charge reaches 35 DEG C, detect LOD with fast tester for water content at 105 DEG C;
(7) dry granulate:
After dried granule crosses 24 eye mesh screens, the above granule of 24 eye mesh screen is weighed;
(8) mixed eventually:
Loaded in mixer by granule after granulate, magnesium stearate is crossed 30 mesh sieves and is entered mixer and mix by following parameters:
Mixing velocity: 15rpm;
Incorporation time: 10 minutes;
(9) granule is unloaded:
Granule after lubrication is installed in bucket or mixer, fastens lid and granule left in hermetic container is medium is ready to use in fill capsule, weigh and calculated yield;
(10) capsule fill:
With capsule and corresponding mould according to theoretical weight fill, directly capsule good for fill is loaded in PE bag;
(11) pack:
Use following parameters capsule is loaded aluminum-plastic packaged in:
Upper heating-up temperature: 120 DEG C;
Lower heating-up temperature: 120 DEG C;
Heat-sealing temperature: 180 DEG C;
Compressed air pressure: 0.8MPa.
3. a kind of Celebret production technology as claimed in claim 2, is characterized in that, in described step (4) during spray granulation solution, can add a small amount of pure water as required.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110604722A (en) * | 2019-09-19 | 2019-12-24 | 山东创新药物研发有限公司 | Solid dispersion method of celecoxib and preparation method of celecoxib capsules |
CN112263562A (en) * | 2020-09-25 | 2021-01-26 | 石药集团欧意药业有限公司 | Preparation method of celecoxib capsule composition |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103372216A (en) * | 2012-04-26 | 2013-10-30 | 北京京卫燕康药物研究所有限公司 | Solid medical composition containing celecoxib |
CN103989657A (en) * | 2013-02-20 | 2014-08-20 | 四川国为制药有限公司 | Celecoxib-containing capsule |
CN104983714A (en) * | 2015-08-06 | 2015-10-21 | 苏州二叶制药有限公司 | Celecoxib capsule and preparing method thereof |
-
2015
- 2015-11-11 CN CN201510770019.9A patent/CN105232494A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103372216A (en) * | 2012-04-26 | 2013-10-30 | 北京京卫燕康药物研究所有限公司 | Solid medical composition containing celecoxib |
CN103989657A (en) * | 2013-02-20 | 2014-08-20 | 四川国为制药有限公司 | Celecoxib-containing capsule |
CN104983714A (en) * | 2015-08-06 | 2015-10-21 | 苏州二叶制药有限公司 | Celecoxib capsule and preparing method thereof |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110604722A (en) * | 2019-09-19 | 2019-12-24 | 山东创新药物研发有限公司 | Solid dispersion method of celecoxib and preparation method of celecoxib capsules |
CN112263562A (en) * | 2020-09-25 | 2021-01-26 | 石药集团欧意药业有限公司 | Preparation method of celecoxib capsule composition |
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