CN1283627A - Process for extracting icariin from epimedium - Google Patents
Process for extracting icariin from epimedium Download PDFInfo
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- CN1283627A CN1283627A CN 00110647 CN00110647A CN1283627A CN 1283627 A CN1283627 A CN 1283627A CN 00110647 CN00110647 CN 00110647 CN 00110647 A CN00110647 A CN 00110647A CN 1283627 A CN1283627 A CN 1283627A
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- TZJALUIVHRYQQB-UHFFFAOYSA-N icariine Natural products C1=CC(OC)=CC=C1C1=C(OC2C(C(O)C(O)C(C)O2)O)C(=O)C2=C(O)C=C(OC3C(C(O)C(O)C(CO)O3)O)C(CC=C(C)C)=C2O1 TZJALUIVHRYQQB-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 13
- 241000893536 Epimedium Species 0.000 title abstract 3
- TZJALUIVHRYQQB-XFDQAQKOSA-N Icariin Natural products O(C)c1ccc(C2=C(O[C@H]3[C@@H](O)[C@H](O)[C@@H](O)[C@H](C)O3)C(=O)c3c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O4)c(C/C=C(\C)/C)c3O2)cc1 TZJALUIVHRYQQB-XFDQAQKOSA-N 0.000 title abstract 2
- 235000018905 epimedium Nutrition 0.000 title abstract 2
- TZJALUIVHRYQQB-XLRXWWTNSA-N icariin Chemical compound C1=CC(OC)=CC=C1C1=C(O[C@H]2[C@@H]([C@H](O)[C@@H](O)[C@H](C)O2)O)C(=O)C2=C(O)C=C(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)C(CC=C(C)C)=C2O1 TZJALUIVHRYQQB-XLRXWWTNSA-N 0.000 title abstract 2
- 239000011347 resin Substances 0.000 claims abstract description 21
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010992 reflux Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 43
- 239000000203 mixture Substances 0.000 claims description 23
- 239000008399 tap water Substances 0.000 claims description 21
- 235000020679 tap water Nutrition 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 14
- 239000002893 slag Substances 0.000 claims description 13
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 238000011084 recovery Methods 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000011010 flushing procedure Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 4
- 238000004061 bleaching Methods 0.000 claims description 2
- 238000005352 clarification Methods 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 8
- 238000001291 vacuum drying Methods 0.000 abstract description 4
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000007921 spray Substances 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 2
- 208000001132 Osteoporosis Diseases 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 201000001881 impotence Diseases 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 206010036596 premature ejaculation Diseases 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
A process for extracting icariin from epimedium includes immersing the epimedium plant over ground in water, decocting, filtering to obtain decoction, vacuum can centrating, adsorption with macroreticular resin, eluting with alcohol, adding medicinal activated carbon, heating, reflux decolouring, recovering alcohol from filtrate, and spray or vacuum drying. Its advantages include no residual organic solvent and no environmental pollution.
Description
The present invention relates to a kind of method of extracting medicine from plant, exactly is a kind of method of extracting icarin from Herba Epimedii.
Herba Epimedii is a kind of physiologically active substance, has enriching yin and nourishing kidney, the effect that strengthens muscles and bones, and can treat impotence and premature ejaculation, and be the good merchantable brand of male health-care, also be simultaneously the important substance of the middle-aged and old osteoporosis of treatment.For a long time, experts and scholars have invented many methods of extracting icarin from the Herba Epimedii plant both at home and abroad, all will use methyl alcohol, chloroform or organic solvents such as chloroform and methanol mixture in large quantities when utilizing these methods to produce icarin.The subject matter that exists when utilizing existing method to extract icarin is: 1, production cost is higher; 2, residual harmful organic solvent in the product; 3, environmental pollution is more serious in the production process.
The objective of the invention is for people provide a kind of novel method of carrying icarin from Herba Epimedii, so that overcome problems of the prior art.
The method of extracting icarin from Herba Epimedii provided by the invention comprises following processing step:
A, raw material are the immersion and the decoction of Herba Epimedii over-ground part
(A) weight ratio by raw material and tap water is 1: 12-16 adds tap water in raw material, and soak at room temperature 0.5-2 hour, then, the mixture heating up to 100 ℃ with both was incubated 2-3 hour, afterwards, and residue obtained liquid;
(B) ratio of weight and number by described raw material and tap water is 1: 6-10 adds tap water in the slag that processing step (A) leaches, and with both mixture heating up to 100 ℃, be incubated 2-2.5 hour after, residue obtained liquid;
(C) ratio of weight and number by described raw material and tap water is 1: 6-10 adds tap water in the slag that processing step (B) leaches, and with both mixture heating up to 100 ℃, be incubated 1.5 hours after, residue obtained liquid;
B, the liquid mixing that will be respectively produce by described each processing step (A), (B), (C) be the back concentrating under reduced pressure together, is 1 until the ratio of its weight and described raw material weight: till the 1-2;
C, absorption, wash-out
Macroporous resin column after making liquid after concentrating by activated processing, icarin in the liquid is adsorbed by resin column, and discard effluent liquid, continue with distilled water with concentrate after the volume ratio of liquid be 0.5-1: 1 ratio is taken the distilled water flushing resin column, is discarded the flushing flow fluid, continuing with concentration is 65% ethanol-eluting resin column, till making absorption icarin thereon by complete wash-out, and collect the reservation elutriant;
D, decolouring
, continue than medical active carbon being added in the described elutriant in itself and described raw materials in part by weight, then its temperature is reduced to 50 ℃, and make it to collect filtrate afterwards by the filtration of clarification plate with both mixed solution reflux 20 minutes for the ratio of 0.4-100;
E, recovery solvent, drying
Solvent in the filtrate that recovery bleaching process D makes, remaining material gets product behind spraying drying or the drying under reduced pressure;
The present invention compared with prior art has the following advantages after realizing: 1, production cost of products is lower; 2, it is residual thoroughly to have eliminated in the product deleterious organic substance; 3, production process environmentally safe.
Below in conjunction with embodiment the present invention is done explanation in further detail.
Embodiment one
A, Herba Epimedii over-ground part soak and decoct
(A) the over-ground part 10kg that gets Herba Epimedii puts into container, adds 12 liters in tap water again in container, soak at room temperature 0.5 hour, and then, the mixture heating up to 100 ℃ with both is incubated 2 hours, afterwards, residue obtained liquid;
(B) in the slag that work step (A) leaches, add 6 liters in tap water, and, be incubated 2 hours both mixture heating up to 100 ℃, afterwards, residue obtained liquid;
(C) in the slag that work step (B) leaches, add 6 liters in tap water, and, be incubated 1.5 hours both mixture heating up to 100 ℃, afterwards, residue obtained liquid;
B, liquid concentration
The back together concentrating under reduced pressure of liquid mixing that to produce by above-mentioned each work step (A), (B), (C) respectively is concentrated into about 20 until it and only is upgraded to;
C, absorption, wash-out
Macroporous resin column after making liquid after concentrating by activated processing, icarin in the liquid is adsorbed by resin column, and discard effluent liquid, use 10 liters of distilled water flushing resin columns again, discard effluent liquid, continuing with concentration is that 65% ethanol cleans resin column, absorption icarin is thereon ended by wash-out fully, and collect elutriant;
D, decolouring
To contain medicinal activated carbon 0.04kg and add in the described elutriant, and continue both mixture heating up were refluxed 20 minutes, the temperature of this mixture is reduced to 50 ℃ then, and makes it to filter by clear slag plate, collects filtrate afterwards;
E, recovery solvent, drying
Recovery process D makes the solvent in the filtrate, and remaining material can obtain the icarin finished product after passing through reduced vacuum drying or spraying drying mode drying.
Embodiment two
The immersion of A, Herba Epimedii over-ground part and decoction
(A) the over-ground part 10kg that gets Herba Epimedii puts into container, adds 14 liters in tap water again in container, soak at room temperature 1.5 hours, and then, the mixture heating up to 100 ℃ with both is incubated 2.5 hours, afterwards, residue obtained liquid;
(B) in the slag that work step (A) leaches, add 8 liters in tap water, and, be incubated 2 hours both mixture heating up to 100 ℃, afterwards, residue obtained liquid;
(C) in the slag that work step (B) leaches, add 8 liters in tap water, and, be incubated 1.5 hours both mixture heating up to 100 ℃, afterwards, residue obtained liquid;
B, liquid concentration
The back together concentrating under reduced pressure of liquid mixing that to produce by above-mentioned each work step (A), (B), (C) respectively is concentrated into about 15 until it and only is upgraded to;
C, absorption, wash-out
Macroporous resin column after making liquid after concentrating by activated processing, icarin in the liquid is adsorbed by resin column, and discard effluent liquid, use 15 liters of distilled water flushing resin columns again, discard effluent liquid, continuing with concentration is that 65% ethanol cleans resin column, absorption icarin is thereon ended by wash-out fully, and collect elutriant;
D, decolouring
0.06kg adds in the described elutriant with medical active carbon, continues both mixture heating up were refluxed 20 minutes, and the temperature of this mixture is reduced to 50 ℃ then, and makes it to filter by clear slag plate, collects filtrate afterwards;
E, recovery solvent, drying
Recovery process D makes the solvent in the filtrate, and remaining material can obtain the icarin finished product after passing through reduced vacuum drying or spraying drying mode drying.
Embodiment three
The immersion of A, Herba Epimedii over-ground part and decoction
(A) the over-ground part 10kg that gets Herba Epimedii puts into container, adds 16 liters in tap water again in container, soak at room temperature 2.0 hours, and then, the mixture heating up to 100 ℃ with both is incubated 3 hours, afterwards, residue obtained liquid;
(B) in the slag that work step (A) leaches, add 10 liters in tap water, and, be incubated 2.5 hours both mixture heating up to 100 ℃, afterwards, residue obtained liquid;
(C) in the slag that work step (B) leaches, add 10 liters in tap water, and, be incubated 1.5 hours both mixture heating up to 100 ℃, afterwards, residue obtained liquid;
B, liquid concentration
The back together concentrating under reduced pressure of liquid mixing that to produce by above-mentioned each work step (A), (B), (C) respectively is concentrated into about 10 until it and only is upgraded to;
C, absorption, wash-out
Macroporous resin column after making liquid after concentrating by activated processing, icarin in the liquid is adsorbed by resin column, and discard effluent liquid, use 20 liters of distilled water flushing resin columns again, discard effluent liquid, continuing with concentration is that 65% ethanol cleans resin column, absorption icarin is thereon ended by wash-out fully, and collect elutriant;
D, decolouring
0.1kg adds in the described elutriant with medical active carbon, continues both mixture heating up were refluxed 20 minutes, and the temperature of this mixture is reduced to 50 ℃ then, and makes it to filter by clear slag plate, collects filtrate afterwards;
E, recovery solvent, drying
Recovery process D makes the solvent in the filtrate, and remaining material can obtain the icarin finished product after passing through reduced vacuum drying or spraying drying mode drying.
Herba Epimedii over-ground part of the present invention is meant stem or the leaf or the cauline leaf mixture of Herba Epimedii.Wherein, the icarin content of stem is lower, and the icarin content of leaf is higher.
Claims (1)
1, a kind of method of from Herba Epimedii, extracting icarin, form by following processing step:
A, raw material are the immersion and the decoction of Herba Epimedii over-ground part;
(A) weight ratio by raw material and tap water is 1: 12-16 adds tap water in raw material, and soak at room temperature 0.5-2 hour, then, the mixture heating up to 100 ℃ with both was incubated 2-3 hour, afterwards, and residue obtained liquid;
(B) ratio of weight and number by described raw material and tap water is 1: 6-10 adds tap water in the slag that processing step (A) leaches, and with both mixture heating up to 100 ℃, be incubated 2-2.5 hour after, residue obtained liquid;
(C) ratio of weight and number by described raw material and tap water is 1: 6-10 adds tap water in the slag that processing step (B) leaches, and with both mixture heating up to 100 ℃, be incubated 1.5 hours after, residue obtained liquid;
B, the one super back concentrating under reduced pressure of liquid mixing that will produce by described each processing step (A), (B), (C) respectively are 1 until the ratio of its weight and described raw material weight: till the 1-2;
C, absorption, wash-out
Macroporous resin column after making liquid after concentrating by activated processing, icarin in the liquid is adsorbed by resin column, and discard effluent liquid, continue with distilled water with concentrate after the volume ratio of liquid be 0.5-1: 1 ratio is taken the distilled water flushing resin column, is discarded the flushing flow fluid, continuing with concentration is 65% ethanol-eluting resin column, till making absorption icarin thereon by complete wash-out, and collect the reservation elutriant;
D, decolouring
In itself and described raw materials in part by weight than being 0.4-1: 100 ratio adds medical active carbon in the described elutriant, continues both mixed solution reflux 20 minutes, then its temperature is reduced to 50 ℃, and makes it to filter by the clarification plate, collects filtrate afterwards;
E, recovery solvent, drying
Solvent in the filtrate that recovery bleaching process D makes, remaining material gets product behind spraying drying or the drying under reduced pressure;
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00110647 CN1283627A (en) | 2000-07-12 | 2000-07-12 | Process for extracting icariin from epimedium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00110647 CN1283627A (en) | 2000-07-12 | 2000-07-12 | Process for extracting icariin from epimedium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1283627A true CN1283627A (en) | 2001-02-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00110647 Pending CN1283627A (en) | 2000-07-12 | 2000-07-12 | Process for extracting icariin from epimedium |
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| Country | Link |
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| CN (1) | CN1283627A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312167C (en) * | 2003-06-05 | 2007-04-25 | 北京科锐多科技有限公司 | Epimedium extract and its production method |
| CN101812100A (en) * | 2010-04-08 | 2010-08-25 | 苏州宝泽堂医药科技有限公司 | Method for preparing icariin |
| CN101845067A (en) * | 2010-05-21 | 2010-09-29 | 甘肃亚兰特种药材饮片生产有限公司 | Preparation method of high-content icariin |
| CN101200743B (en) * | 2007-12-17 | 2010-12-15 | 北京珅奥基医药科技有限公司 | Method for preparing hydrated icaritin |
| CN101669980B (en) * | 2008-09-09 | 2011-08-17 | 劲牌有限公司 | Method for extracting and separating icariin and flavone from epimedium herb |
| CN102718819A (en) * | 2012-07-10 | 2012-10-10 | 刘志强 | Process for preparing icariin |
| CN101747391B (en) * | 2008-12-17 | 2013-01-02 | 中国科学院大连化学物理研究所 | Method for separating and preparing chemical reference substance of Icariin |
| CN103288900A (en) * | 2013-05-13 | 2013-09-11 | 张洋 | Icariin preparation process flow |
| CN103396463A (en) * | 2013-08-22 | 2013-11-20 | 内蒙古鑫吉利生物科技有限公司 | Method for extracting icariin from epimedium |
| CN103910772A (en) * | 2014-04-18 | 2014-07-09 | 成都合盛生物技术有限公司 | Method for simultaneously extracting icariin and baohuoside I and II from herba epimedii |
| CN104059116A (en) * | 2014-04-30 | 2014-09-24 | 西安岳达植物科技有限公司 | Method for separating icariine from herba epimedii |
| CN107973829A (en) * | 2017-12-18 | 2018-05-01 | 四川合盛生物科技有限公司 | A kind of method that icariin is extracted from Herba Epimedii |
-
2000
- 2000-07-12 CN CN 00110647 patent/CN1283627A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312167C (en) * | 2003-06-05 | 2007-04-25 | 北京科锐多科技有限公司 | Epimedium extract and its production method |
| CN101200743B (en) * | 2007-12-17 | 2010-12-15 | 北京珅奥基医药科技有限公司 | Method for preparing hydrated icaritin |
| CN101669980B (en) * | 2008-09-09 | 2011-08-17 | 劲牌有限公司 | Method for extracting and separating icariin and flavone from epimedium herb |
| CN101747391B (en) * | 2008-12-17 | 2013-01-02 | 中国科学院大连化学物理研究所 | Method for separating and preparing chemical reference substance of Icariin |
| CN101812100A (en) * | 2010-04-08 | 2010-08-25 | 苏州宝泽堂医药科技有限公司 | Method for preparing icariin |
| CN101845067A (en) * | 2010-05-21 | 2010-09-29 | 甘肃亚兰特种药材饮片生产有限公司 | Preparation method of high-content icariin |
| CN102718819A (en) * | 2012-07-10 | 2012-10-10 | 刘志强 | Process for preparing icariin |
| CN102718819B (en) * | 2012-07-10 | 2013-07-03 | 刘志强 | Process for preparing icariin |
| CN103288900A (en) * | 2013-05-13 | 2013-09-11 | 张洋 | Icariin preparation process flow |
| CN103396463A (en) * | 2013-08-22 | 2013-11-20 | 内蒙古鑫吉利生物科技有限公司 | Method for extracting icariin from epimedium |
| CN103396463B (en) * | 2013-08-22 | 2016-05-18 | 内蒙古鑫吉利生物科技有限公司 | A kind of method of extracting icariin from barrenwort |
| CN103910772A (en) * | 2014-04-18 | 2014-07-09 | 成都合盛生物技术有限公司 | Method for simultaneously extracting icariin and baohuoside I and II from herba epimedii |
| CN103910772B (en) * | 2014-04-18 | 2015-11-18 | 成都合盛生物技术有限公司 | A kind of method simultaneously extracting icarin and the precious leaves of pulse plants glycosides I, II from Herba Epimedii |
| CN104059116A (en) * | 2014-04-30 | 2014-09-24 | 西安岳达植物科技有限公司 | Method for separating icariine from herba epimedii |
| CN107973829A (en) * | 2017-12-18 | 2018-05-01 | 四川合盛生物科技有限公司 | A kind of method that icariin is extracted from Herba Epimedii |
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