CN103952240A - Preparation method of abelmoschus manihot essential oil - Google Patents
Preparation method of abelmoschus manihot essential oil Download PDFInfo
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- CN103952240A CN103952240A CN201410212474.2A CN201410212474A CN103952240A CN 103952240 A CN103952240 A CN 103952240A CN 201410212474 A CN201410212474 A CN 201410212474A CN 103952240 A CN103952240 A CN 103952240A
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 240000005959 Abelmoschus manihot Species 0.000 title abstract description 9
- 235000001075 Abelmoschus manihot Nutrition 0.000 title abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000004821 distillation Methods 0.000 claims abstract description 9
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 239000003921 oil Substances 0.000 claims abstract description 9
- 238000010992 reflux Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 5
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 5
- 230000018044 dehydration Effects 0.000 claims abstract description 4
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 239000002274 desiccant Substances 0.000 claims abstract description 3
- 241001075517 Abelmoschus Species 0.000 claims description 39
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- 241000628997 Flos Species 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 235000005739 manihot Nutrition 0.000 claims description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 244000149260 Manihot esculenta subsp flabellifolia Species 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 150000004676 glycans Chemical class 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 229920001282 polysaccharide Polymers 0.000 abstract description 4
- 239000005017 polysaccharide Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 206010062717 Increased upper airway secretion Diseases 0.000 abstract 1
- 238000011049 filling Methods 0.000 abstract 1
- 239000000499 gel Substances 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 208000026435 phlegm Diseases 0.000 abstract 1
- 238000000034 method Methods 0.000 description 7
- 239000003292 glue Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical compound C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 description 2
- REPVLJRCJUVQFA-UHFFFAOYSA-N (-)-isopinocampheol Natural products C1C(O)C(C)C2C(C)(C)C1C2 REPVLJRCJUVQFA-UHFFFAOYSA-N 0.000 description 2
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 2
- 241000723346 Cinnamomum camphora Species 0.000 description 2
- 241000221022 Manihot Species 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- CKDOCTFBFTVPSN-UHFFFAOYSA-N borneol Natural products C1CC2(C)C(C)CC1C2(C)C CKDOCTFBFTVPSN-UHFFFAOYSA-N 0.000 description 2
- 229940116229 borneol Drugs 0.000 description 2
- 229930008380 camphor Natural products 0.000 description 2
- 229960000846 camphor Drugs 0.000 description 2
- 229930002875 chlorophyll Natural products 0.000 description 2
- 235000019804 chlorophyll Nutrition 0.000 description 2
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 2
- DTGKSKDOIYIVQL-UHFFFAOYSA-N dl-isoborneol Natural products C1CC2(C)C(O)CC1C2(C)C DTGKSKDOIYIVQL-UHFFFAOYSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- 241001573881 Corolla Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241000219071 Malvaceae Species 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 208000025865 Ulcer Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical class CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 210000005095 gastrointestinal system Anatomy 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 229930006721 pinocarveol Natural products 0.000 description 1
- LCYXQUJDODZYIJ-UHFFFAOYSA-N pinocarveol Chemical compound C1C2C(C)(C)C1CC(O)C2=C LCYXQUJDODZYIJ-UHFFFAOYSA-N 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 231100000397 ulcer Toxicity 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000011345 viscous material Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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- Fats And Perfumes (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of essential oil and in particular relates to a preparation method of abelmoschus manihot essential oil. The preparation method comprises the steps of grinding abelmoschus manihot dried in the shade into powder; wrapping the abelmoschus manihot powder with filter paper, putting the abelmoschus manihot powder in an extractor, adding a low-boiling-point solvent, heating the solvent to carry out reflux and repeated extraction until the solvent is colorless, and cooling and collecting the extracting solution; concentrating the extracting solution to volatize all the solvent; filling the abelmoschus manihot extract with all the solvent volatized into the extractor, adding distilled water, shaking the extractor to mix the abelmoschus manihot extract with the distilled water, connecting with a reflux condensing tube, carrying out heating distillation until the essential oil in the extractor is no longer added, and cooling and collecting the oil layer; adding an inorganic salt drying agent to the oil layer for dehydration, and sealing for storing, thus obtaining the abelmoschus manihot essential oil. The preparation method has the beneficial effects that firstly the low-boiling-point organic solvent is heated to undergo continuous reflux extraction, thus avoiding inference of substances such as gels, phlegm, polysaccharides and the like; non-volatile impurities are removed by distilling the extract and water; the organic solvent is volatized at low temperature before distillation, thus avoiding the residues of the solvent.
Description
Technical field
The present invention relates to a kind of volatile oil extractive technique field, specifically a kind of preparation method of Flower of Sunset Abelmoschus volatile oil.
Background technology
Flower of Sunset Abelmoschus is the dry corolla of Malvaceae plant Abelmoschus manihot (L.) Medic..2010 editions " Chinese Pharmacopoeias " record, and have damp-excreting medicinal clearly, and subduing swelling and detoxicating effect is held back for damp and hot heap soil or fertilizer over and around the roots, stranguria with turbid discharge oedema; Control swollen ulcer drug outward, burn due to hot liquid or fire etc.Song dynasty " good help book on Chinese herbal medicine ": control urine leaching and expedite the emergence of, main all evil sore pus person that is not recovered for a long time, does end and apply again.Ming Dynasty's Compendium of Material Medica: subduing inflammation, immersion oil is coated with burn.Extensive artificial culture at present, more to flavonoid in Flower of Sunset Abelmoschus, polysaccharose substance research, less to volatile oil research contained in spending.
The extracting method of volatile oil has a variety of, mainly contains steam distillation, solvent-extraction process, supercritical fluid extraction etc.Because Flower of Sunset Abelmoschus contains a large amount of Sunset Abelmoschus Root glue, phlegmatic temperament, polysaccharide etc., chance water stripping makes solution thickness, and heating is easily charred, and affects the extraction of volatile oil; Use separately solvent-extraction process, contain the impurity such as a large amount of resins, grease, wax, chlorophyll.
At present fragrant volatile oil contained in Flower of Sunset Abelmoschus is extracted to research seldom.Only have in the recent period one section (Zhang Yuanyuan, Jia Xiaoni, Cao Yongxiang, etc.Flower of Sunset Abelmoschus chemical constitution study [J], northwest pharmaceutical journal, 2008,23 (2): 80-82) what adopt is wet distillation, but find through actual verification, after Flower of Sunset Abelmoschus is met water, tackiness increases, and heat is just black a little.
Summary of the invention
In order to overcome the shortcoming part existing in above-mentioned prior art, the technical problem to be solved in the present invention is to provide a kind of preparation method of Flower of Sunset Abelmoschus volatile oil.
To achieve these goals, the technical solution adopted in the present invention is: a kind of preparation method of Flower of Sunset Abelmoschus volatile oil, and step is as follows:
1), the Flower of Sunset Abelmoschus drying in the shade is pulverized and is powdery;
2), continuous circumfluence extraction
With filter paper parcel Flower of Sunset Abelmoschus powder, and be placed in extractor, add low boiling point solvent, 40～60 DEG C of reflux are repeatedly extracted into solvent and are colourless, cooling, collection extracting solution;
3), extracting solution is placed at 20～40 DEG C and concentrates and wave most solvent;
4), water distillation altogether
The Flos abelmoschi manihot extract of waving most solvent is packed in extractor, add distilled water jolting to mix, connect reflux condensing tube, heating is distilled to volatile oil in extractor no longer to be increased, cooling, collection oil reservoir;
5), in oil reservoir, add inorganic salt desiccant dehydration, sealing is preserved, and obtains Flower of Sunset Abelmoschus volatile oil.
Preferably, described step 1) in the fineness of powdery Flower of Sunset Abelmoschus be 10～80 orders.
Preferably, described step 2) in extractor be cable type extractor according.
Preferably, described step 2) in low boiling point solvent be ether.
Preferably, described step 4) in extractor be volatile oil extractor.
Preferably, described step 5) in inorganic salt siccative be anhydrous sodium sulphate.
The preparation method of Flower of Sunset Abelmoschus volatile oil of the present invention, its beneficial effect is embodied in:
1), the present invention contains a large amount of phlegmatic temperaments, colloid etc. according to Flower of Sunset Abelmoschus, have the advantages that to meet the stripping of glue viscous substance, adopt and first use low boiling point organic solvent continuous circumfluence extraction, extract prepares Flower of Sunset Abelmoschus volatile oil with being total to water distillating method again.Meanwhile, owing to first heating continuous circumfluence extraction with low boiling point organic solvent, avoided the material such as glue class, phlegmatic temperament, polysaccharide to disturb, the extract distillation that adds water again, to have removed involatile constituent.Through gas chromatography combined with mass spectrometry (GC-MS), first identified goes out in Flower of Sunset Abelmoschus volatile oil, mainly to contain aromatoising substance and the active substances such as β-Se Lin alkene, camphor, borneol.
2), the invention solves Flower of Sunset Abelmoschus can not be by the problem of water extraction volatile oil, Flower of Sunset Abelmoschus contains a large amount of Sunset Abelmoschus Root glue, phlegmatic temperament, polysaccharide etc., meet water stripping make solution thickness, affect the extraction of volatile oil, heat and be easily charred.Meanwhile, if use separately solvent-extraction process, easily contain the impurity such as a large amount of resins, grease, wax, chlorophyll.The present invention, by extract water distillation altogether, has removed non-volatile impurities.Before distillation, low temperature is flung to organic solvent, has avoided the residual of solvent.
3), whole leaching process temperature is not high, heat-up time is short, has avoided in volatile oil the thermo-labile component destruction that is decomposed.
4), mostly volatile oil is small-molecule substance, can be absorbed fast by body, effect extensively, cardio-cerebrovascular, central nervous system, respiratory system, gastrointestinal system, antibacterial, anti-inflammatory, anticancer, antiviral, promote the many-sides such as drug absorption all to there is effect.The invention solves current Flower of Sunset Abelmoschus volatile oil and extract the defect existing, for the further investigation of Flower of Sunset Abelmoschus volatile oil, disclose its mechanism of action, Application and Development etc. are laid a good foundation.
Brief description of the drawings
Fig. 1 is the GC-MS total ion current figure of the Flower of Sunset Abelmoschus volatile oil prepared of the embodiment of the present invention.
In figure:
1. camphor 2. borneol
3. β-Se Lin alkene 4.10s, 11s-Himachala-3 (12) 4-diene
5. trans-long pinocarveol 6. dibutyl phthalates
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated, but the present invention is not limited only to embodiment, under the prerequisite that does not depart from aim of the present invention, within any improvement of doing all drops on protection scope of the present invention.
The preparation method of Flower of Sunset Abelmoschus volatile oil, step is as follows:
1), the Flower of Sunset Abelmoschus drying in the shade being crushed to fineness is 10～80 object powderies.
2), continuous circumfluence extraction
With filter paper parcel Flower of Sunset Abelmoschus powder, and be placed in cable type extractor according, add ether, 40～60 DEG C of reflux are repeatedly extracted into solvent and are colourless, cooling, collection extracting solution.
3), extracting solution is placed at 20～40 DEG C and concentrates and wave most solvent.
4), water distillation altogether
The Flos abelmoschi manihot extract of waving most solvent is packed in volatile oil extractor, add distilled water jolting to mix, connect reflux condensing tube, heating is distilled to volatile oil in volatile oil extractor no longer to be increased, cooling, collection oil reservoir.
5), in oil reservoir, add anhydrous sodium sulfate dehydration, sealing is preserved, and obtains the Flower of Sunset Abelmoschus volatile oil as shown in Fig. 1 collection of illustrative plates.
Above content is only to structure example of the present invention and explanation; affiliated those skilled in the art make various amendments to described specific embodiment or supplement or adopt similar mode to substitute; only otherwise depart from the structure of invention or surmount this scope as defined in the claims, all should belong to protection scope of the present invention.
Claims (6)
1. a preparation method for Flower of Sunset Abelmoschus volatile oil, is characterized in that step is as follows:
1), the Flower of Sunset Abelmoschus drying in the shade is pulverized and is powdery;
2), continuous circumfluence extraction
With filter paper parcel Flower of Sunset Abelmoschus powder, and be placed in extractor, add low boiling point solvent, 40～60 DEG C of reflux are repeatedly extracted into solvent and are colourless, cooling, collection extracting solution;
3), extracting solution is placed at 20～40 DEG C and concentrates and wave most solvent;
4), water distillation altogether
The Flos abelmoschi manihot extract of waving most solvent is packed in extractor, add distilled water jolting to mix, connect reflux condensing tube, heating is distilled to volatile oil in extractor no longer to be increased, cooling, collection oil reservoir;
5), in oil reservoir, add inorganic salt desiccant dehydration, sealing is preserved, and obtains Flower of Sunset Abelmoschus volatile oil.
2. the preparation method of Flower of Sunset Abelmoschus volatile oil according to claim 1, is characterized in that: described step 1) in the fineness of powdery Flower of Sunset Abelmoschus be 10～80 orders.
3. the preparation method of Flower of Sunset Abelmoschus volatile oil according to claim 1, is characterized in that: described step 2) in extractor be cable type extractor according.
4. the preparation method of Flower of Sunset Abelmoschus volatile oil according to claim 1, is characterized in that: described step 2) in low boiling point solvent be ether.
5. the preparation method of Flower of Sunset Abelmoschus volatile oil according to claim 1, is characterized in that: described step 4) in extractor be volatile oil extractor.
6. the preparation method of Flower of Sunset Abelmoschus volatile oil according to claim 1, is characterized in that: described step 5) in inorganic salt siccative be anhydrous sodium sulphate.
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| CN201410212474.2A CN103952240B (en) | 2014-05-19 | 2014-05-19 | A kind of preparation method of Flower of Sunset Abelmoschus volatile oil |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104178350A (en) * | 2014-08-18 | 2014-12-03 | 安徽科技学院 | Method for separating and extracting chrysanthemum volatile oil, fiavonoid and phenolic acids from chrysanthemum |
| CN105362311A (en) * | 2015-11-23 | 2016-03-02 | 安徽科技学院 | Method for extracting and separating volatile oil, flavone and polysaccharide of abelmoschus manihot flowers |
| CN106138315A (en) * | 2016-08-09 | 2016-11-23 | 许备占 | Wild lotus lozenge and preparation method thereof |
| CN106244325A (en) * | 2016-08-16 | 2016-12-21 | 重庆雅香美源生态农业科技有限公司 | The extraction of a kind of Herba Acroptili repentis quintessence oil and processing method |
| CN108424815A (en) * | 2018-05-29 | 2018-08-21 | 安徽安亳食品有限公司 | A kind of preparation method of okra essential oil |
| CN109090702A (en) * | 2018-06-29 | 2018-12-28 | 郑州轻工业学院 | The preparation method and applications of Luo Han Guo Paste In Foods maillard reaction product |
| CN109897730A (en) * | 2019-03-18 | 2019-06-18 | 黑龙江中医药大学 | A kind of Du Xiang refined volatile oil refinement method |
| CN111849643A (en) * | 2020-07-28 | 2020-10-30 | 福建省建瓯市金路实业有限公司 | Distillation extraction method of cedar oil |
| CN115851378A (en) * | 2022-12-05 | 2023-03-28 | 吉林省林业科学研究院 | Extraction method of phellodendron amurense fruit essential oil |
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| CN107629874A (en) * | 2017-10-10 | 2018-01-26 | 广东长利香精香料有限公司 | A kind of cinnamomum camphora Verbena officinalis essential oil |
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Cited By (10)
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| CN104178350A (en) * | 2014-08-18 | 2014-12-03 | 安徽科技学院 | Method for separating and extracting chrysanthemum volatile oil, fiavonoid and phenolic acids from chrysanthemum |
| CN105362311A (en) * | 2015-11-23 | 2016-03-02 | 安徽科技学院 | Method for extracting and separating volatile oil, flavone and polysaccharide of abelmoschus manihot flowers |
| CN106138315A (en) * | 2016-08-09 | 2016-11-23 | 许备占 | Wild lotus lozenge and preparation method thereof |
| CN106244325A (en) * | 2016-08-16 | 2016-12-21 | 重庆雅香美源生态农业科技有限公司 | The extraction of a kind of Herba Acroptili repentis quintessence oil and processing method |
| CN108424815A (en) * | 2018-05-29 | 2018-08-21 | 安徽安亳食品有限公司 | A kind of preparation method of okra essential oil |
| CN109090702A (en) * | 2018-06-29 | 2018-12-28 | 郑州轻工业学院 | The preparation method and applications of Luo Han Guo Paste In Foods maillard reaction product |
| CN109090702B (en) * | 2018-06-29 | 2021-08-24 | 郑州轻工业学院 | Preparation method and application of Maillard reaction product of fructus momordicae extract |
| CN109897730A (en) * | 2019-03-18 | 2019-06-18 | 黑龙江中医药大学 | A kind of Du Xiang refined volatile oil refinement method |
| CN111849643A (en) * | 2020-07-28 | 2020-10-30 | 福建省建瓯市金路实业有限公司 | Distillation extraction method of cedar oil |
| CN115851378A (en) * | 2022-12-05 | 2023-03-28 | 吉林省林业科学研究院 | Extraction method of phellodendron amurense fruit essential oil |
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| CN103952240B (en) | 2015-09-30 |
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