CN102040548A - Method for extracting beta-carotene and zeaxanthin from Chinese wolfberry skin - Google Patents
Method for extracting beta-carotene and zeaxanthin from Chinese wolfberry skin Download PDFInfo
- Publication number
- CN102040548A CN102040548A CN2010105737745A CN201010573774A CN102040548A CN 102040548 A CN102040548 A CN 102040548A CN 2010105737745 A CN2010105737745 A CN 2010105737745A CN 201010573774 A CN201010573774 A CN 201010573774A CN 102040548 A CN102040548 A CN 102040548A
- Authority
- CN
- China
- Prior art keywords
- elutriant
- medicinal extract
- zeaxanthin
- chinese wolfberry
- sherwood oil
- 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.)
- Pending
Links
Abstract
The invention discloses a method for extracting beta-carotene and zeaxanthin from Chinese wolfberry skin. The method comprises the following steps: (1) extraction: drying and crashing Chinese wolfberry skin, adding mixed solvent, adding antioxidant, stirring, extracting and performing vacuum concentration on extracting solution under reduced pressure to obtain extractum; (2) saponification: adding petroleum ether to dissolve, adding sodium hydroxide-methanol solution, performing cold process for soap, layering with a separatory funnel and washing ether layer with water to remove sodium hydroxide; (3) purification; and (4) adopting high performance liquid chromatography for treatment, and drying the collected eluent 1 and eluent 2 respectively under reduced pressure to obtain extractum. In the invention, the waste Chinese wolfberry skin generated in the production processes of Chinese Wolfberry juice and Chinese Wolfberry wine can be fully used as the raw material, thus the pollution to the environment can be reduced; and the purity of beta-carotene is up to 10% and the purity of zeaxanthin is up to 65%.
Description
Technical field
The invention belongs to the extracting method of β-Hu Luobusu, zeaxanthin, particularly relate to a kind of method of from matrimony vine skin slag, extracting β-Hu Luobusu, zeaxanthin.
Background technology
β-Hu Luobusu, zeaxanthin belong to poly-penta 2 hydrocarbon compounds, belong to carotenoids, and modern pharmacology research thinks that carotenoid has the enhancing immunity function, prevents atherosclerosis and anticancer, the anti-ageing effect of waiting for a long time.
Structural formula is as follows
Structural formula one is that zeaxanthin, structural formula two are β-Hu Luobusu
Structural formula one
Structural formula two
In foodstuffs industry fast development, today with rapid changepl. never-ending changes and improvements, people have proposed new standard to the requirement of food dye.Though synthetic colour is bright in colour, good stability is cheap, because of synthetic toxicity problem, people is worried and fear; Meanwhile, natural green plant pigments safety non-toxic, and its distinctive nutritive value and physiologically active, be loved by the people, pigment in the matrimony vine is rich in abundant carotenoid, and therefore, wolfberry pigment is all having bright development prospect aspect foodstuffs industry and the medicines and health protection.
Matrimony vine juice and Lycium chinense wine are to be the product of raw material production with matrimony vine, in the process of producing these products, produce a large amount of byproduct residue---matrimony vine skin slag, abandoning these byproducts can pollute environment.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of method of extracting β-Hu Luobusu, zeaxanthin from matrimony vine skin slag is provided.
Technical scheme of the present invention is summarized as follows:
From matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, comprise the steps:
(1) extracts: matrimony vine skin slag drying, pulverizing, with the feed liquid mass ratio is that 1: 15～20 ratio adds mixed solvent and gets mixing liquid, the antioxidant 2 that adds mixing liquid quality 0.1%～0.3%, the anti-sepsis acid of 6-ditertbutylparacresol or 0.3%-0.5%, stirred 1～2 hour, extract twice, united extraction liquid is condensed into medicinal extract with described extracting solution vacuum decompression; Described mixed solvent is that volume ratio is 1: 1～4 hexanaphthene and acetone;
(2) saponification: in described medicinal extract, add sherwood oil, the mass ratio of described medicinal extract and sherwood oil is 1: 1～4, medicinal extract is all dissolved, add mass percent again and be 15%～40% sodium hydrate methanol solution, the mass ratio of described medicinal extract and described sodium hydrate methanol solution 1: 2～5 is placed on the cold soap of shady place 10～24 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, is that 1～4: 1 the sherwood oil and the mixed solvent of acetone carry out gradient elution with sherwood oil, volume ratio, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 85: 15～80: 20; Flow velocity is 0.7～1.0ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, elutriant 1 and the elutriant of collecting 2 is carried out drying under reduced pressure respectively to medicinal extract, again oven dry.
Advantage of the present invention is:
It is raw material that the present invention can make full use of the depleted matrimony vine skin slag that produces in matrimony vine juice and the Lycium chinense wine production process, reduces its pollution to environment, and the β-Hu Luobusu purity of utilizing method of the present invention to extract can reach 10%, zeaxanthin purity can reach 65%.Carotenoid such as β-Hu Luobusu, zeaxanthin need be finished extraction separation in the short period of time to light, heat and air-sensitive, method of the present invention is extracted fast, has improved the extraction yield of β-Hu Luobusu, zeaxanthin.The elutriant 1 collected and elutriant 2 are carried out with drying under reduced pressure to medicinal extract, and oven dry promptly gets product
Embodiment:
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
From matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, comprise the steps:
(1) with matrimony vine skin slag drying, pulverizing, with the feed liquid mass ratio is that 1: 18 ratio adds mixed solvent and gets mixing liquid, the antioxidant 2 that adds mixing liquid quality 0.1%, the 6-ditertbutylparacresol, stirred 1 hour, extract twice, united extraction liquid is condensed into medicinal extract with the extracting solution vacuum decompression; Mixed solvent is that volume ratio is 1: 2 hexanaphthene and an acetone;
(2) saponification: in medicinal extract, add sherwood oil, the mass ratio of medicinal extract and sherwood oil is 1: 2, medicinal extract is all dissolved, add mass percent again and be 20% sodium hydrate methanol solution, the mass ratio of medicinal extract and sodium hydrate methanol solution 1: 3 is placed on the cold soap of shady place 15 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, with sherwood oil, volume ratio be 1: 1,2: 1,3: 1,4: 1, sherwood oil and the mixed solvent of acetone carry out gradient elution, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 85: 15; Flow velocity is 1.0ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, elutriant 1 and the elutriant of collecting 2 is carried out drying under reduced pressure respectively to medicinal extract, again oven dry.
Embodiment 2
From matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, comprise the steps:
(1) with matrimony vine skin slag drying, pulverizing, be that 1: 15 ratio adds mixed solvent and gets mixing liquid with the feed liquid mass ratio, add the anti-sepsis acid of antioxidant of mixing liquid quality 0.5%, stirred 2 hours, extract twice, united extraction liquid is condensed into medicinal extract with the extracting solution vacuum decompression; Mixed solvent is that volume ratio is 1: 3 hexanaphthene and an acetone;
(2) saponification: in medicinal extract, add sherwood oil, the mass ratio of medicinal extract and sherwood oil is 1: 3, medicinal extract is all dissolved, add mass percent again and be 30% sodium hydrate methanol solution, the mass ratio of medicinal extract and sodium hydrate methanol solution 1: 4 is placed on the cold soap of shady place 18 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, with sherwood oil, volume ratio be 1: 1,2: 1,3: 1,4: 1, sherwood oil and the mixed solvent of acetone carry out gradient elution, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 80: 20; Flow velocity is 1.0ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, elutriant 1 and the elutriant of collecting 2 is carried out drying under reduced pressure respectively to medicinal extract, again oven dry.
Embodiment 3
From matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, comprise the steps:
(1) with matrimony vine skin slag drying, pulverizing, with the feed liquid mass ratio is that 1: 20 ratio adds mixed solvent and gets mixing liquid, the antioxidant 2 that adds mixing liquid quality 0.3%, the 6-ditertbutylparacresol, stirred 1 hour, extract twice, united extraction liquid is condensed into medicinal extract with the extracting solution vacuum decompression; Mixed solvent is that volume ratio is 1: 1 hexanaphthene and an acetone;
(2) saponification: in medicinal extract, add sherwood oil, the mass ratio of medicinal extract and sherwood oil is 1: 1, medicinal extract is all dissolved, add mass percent again and be 15% sodium hydrate methanol solution, the mass ratio of medicinal extract and sodium hydrate methanol solution 1: 5 is placed on the cold soap of shady place 10 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, with sherwood oil, volume ratio be 1: 1,2: 1,3: 1,4: 1, sherwood oil and the mixed solvent of acetone carry out gradient elution, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 85: 15; Flow velocity is 0.8ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, elutriant 1 and the elutriant of collecting 2 is carried out drying under reduced pressure respectively to medicinal extract, again oven dry.
Embodiment 4
From matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, comprise the steps:
(1) with matrimony vine skin slag drying, pulverizing, be that 1: 19 ratio adds mixed solvent and gets mixing liquid with the feed liquid mass ratio, add the anti-sepsis acid of antioxidant of mixing liquid quality 0.3%, stirred 2 hours, extract twice, united extraction liquid is condensed into medicinal extract with the extracting solution vacuum decompression; Mixed solvent is that volume ratio is 1: 4 hexanaphthene and an acetone;
(2) saponification: in medicinal extract, add sherwood oil, the mass ratio of medicinal extract and sherwood oil is 1: 4, medicinal extract is all dissolved, add mass percent again and be 40% sodium hydrate methanol solution, the mass ratio of medicinal extract and sodium hydrate methanol solution 1: 2 is placed on the cold soap of shady place 24 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, with sherwood oil, volume ratio be 1: 1,2: 1,3: 1,4: 1, sherwood oil and the mixed solvent of acetone carry out gradient elution, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 80: 20; Flow velocity is 0.9ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, elutriant 1 and the elutriant of collecting 2 is carried out drying under reduced pressure respectively to medicinal extract, again oven dry.
Embodiment 5
Step (2) saponification as different from Example 1: employing be not cold soap, but hot soap is 85 ℃ of water-baths heating 35min in temperature, other step and parameter are with embodiment 1.
Embodiment 6:
As different from Example 1 at step (3) purifying: silicagel column carries out liquid phase adsorption separation on the ether layer after the saponification, and other steps and parameter are with embodiment 1.
By comparing embodiment 1,2,3,4,5,6, four embodiment in front, effect is better, and extraction yield is big.β-Hu Luobusu purity can reach more than 10%, zeaxanthin purity can reach 65 above %.。
Claims (1)
1. from matrimony vine skin slag, extract the method for β-Hu Luobusu, zeaxanthin, it is characterized in that comprising the steps:
(1) extracts: matrimony vine skin slag drying, pulverizing, with the feed liquid mass ratio is that 1: 15～20 ratio adds mixed solvent and gets mixing liquid, the antioxidant 2 that adds mixing liquid quality 0.1%～0.3%, the anti-sepsis acid of 6-ditertbutylparacresol or 0.3%-0.5%, stirred 1～2 hour, extract twice, united extraction liquid is condensed into medicinal extract with described extracting solution vacuum decompression; Described mixed solvent is that volume ratio is 1: 1～4 hexanaphthene and acetone;
(2) saponification: in described medicinal extract, add sherwood oil, the mass ratio of described medicinal extract and sherwood oil is 1: 1～4, medicinal extract is all dissolved, add mass percent again and be 15%～40% sodium hydrate methanol solution, the mass ratio of described medicinal extract and described sodium hydrate methanol solution 1: 2～5 is placed on the cold soap of shady place 10～24 hours, the separating funnel layering, the ether layer washes with water, removes sodium hydroxide;
(3) purifying: magnesium oxide post on the ether layer after the saponification is carried out liquid phase adsorption separation, is that 1～4: 1 the sherwood oil and the mixed solvent of acetone carry out gradient elution with sherwood oil, volume ratio, elutriant 1 and elutriant 2;
(4) high performance liquid chromatography: chromatographic condition is C18 chromatographic column: 250mm * 4.6mm; Moving phase: acetonitrile-methyl alcohol 85: 15～80: 20; Flow velocity is 0.7～1.0ml/min; The detection wavelength is λ=450nm; Sample size is that 20 μ l column temperatures are 25 ℃; Measuring elutriant 1 through the HPLC Liquid Detection is that β-Hu Luobusu elutriant 2 is zeaxanthin, and elutriant 1 and the elutriant of collecting 2 carried out drying under reduced pressure respectively to medicinal extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105737745A CN102040548A (en) | 2010-12-09 | 2010-12-09 | Method for extracting beta-carotene and zeaxanthin from Chinese wolfberry skin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105737745A CN102040548A (en) | 2010-12-09 | 2010-12-09 | Method for extracting beta-carotene and zeaxanthin from Chinese wolfberry skin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102040548A true CN102040548A (en) | 2011-05-04 |
Family
ID=43907122
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105737745A Pending CN102040548A (en) | 2010-12-09 | 2010-12-09 | Method for extracting beta-carotene and zeaxanthin from Chinese wolfberry skin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102040548A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288716A (en) * | 2011-05-12 | 2011-12-21 | 云南农业大学 | Method for testing residual canthaxanthin in animal body |
| CN102886153A (en) * | 2012-10-24 | 2013-01-23 | 周学义 | Method for extracting eyesight improving functional components in Chinese wolfberries and dregs thereof |
| CN103130698A (en) * | 2011-12-01 | 2013-06-05 | 周学义 | Method extracting maize yellow from medlar and medlar dregs |
| CN103149165A (en) * | 2013-01-28 | 2013-06-12 | 西北农林科技大学 | Orange cabbage carotenoid extracting and measuring method |
| WO2013123618A1 (en) * | 2012-02-22 | 2013-08-29 | Dsm Ip Assets B.V. | Process for manufacture of extract containing zeaxanthin and/or its esters |
| CN103504435A (en) * | 2013-10-13 | 2014-01-15 | 全亚平 | Zeaxanthin-rich eyesight-improving wolfberry beverage and production method thereof |
| CN104803901A (en) * | 2014-01-27 | 2015-07-29 | 中国科学院大连化学物理研究所 | Method for preparing zeaxanthin through in situ enrichment |
| CN106093264A (en) * | 2016-07-20 | 2016-11-09 | 福建省农业科学院作物研究所 | A kind of assay method of Fructus Fragariae Ananssae Xanthophyll Cycle Components |
| CN107141841A (en) * | 2017-07-04 | 2017-09-08 | 江苏食品药品职业技术学院 | A kind of wolfberry pigment product and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003020053A1 (en) * | 2001-09-04 | 2003-03-13 | Lycored Natural Products Industries Ltd. | Carotenoid extraction process |
-
2010
- 2010-12-09 CN CN2010105737745A patent/CN102040548A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003020053A1 (en) * | 2001-09-04 | 2003-03-13 | Lycored Natural Products Industries Ltd. | Carotenoid extraction process |
Non-Patent Citations (2)
| Title |
|---|
| 冯作山等: "枸杞色素的提取及纯化技术", 《食品与发酵工业》, vol. 30, no. 12, 31 December 2004 (2004-12-31), pages 141 - 143 * |
| 李赫: "枸杞类胡萝卜素的分析方法及其加工过程中变化的研究", 《中国农业大学硕士学位论文》, 20 June 2006 (2006-06-20) * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102288716A (en) * | 2011-05-12 | 2011-12-21 | 云南农业大学 | Method for testing residual canthaxanthin in animal body |
| CN103130698A (en) * | 2011-12-01 | 2013-06-05 | 周学义 | Method extracting maize yellow from medlar and medlar dregs |
| CN104136035A (en) * | 2012-02-22 | 2014-11-05 | 帝斯曼知识产权资产管理有限公司 | Process for manufacture of extract containing zeaxanthin and/or its esters |
| CN104136035B (en) * | 2012-02-22 | 2019-01-01 | 帝斯曼知识产权资产管理有限公司 | The method for manufacturing the extract containing zeaxanthin and/or its ester |
| WO2013123618A1 (en) * | 2012-02-22 | 2013-08-29 | Dsm Ip Assets B.V. | Process for manufacture of extract containing zeaxanthin and/or its esters |
| CN102886153B (en) * | 2012-10-24 | 2015-12-02 | 周学义 | The extracting method of improving eyesight functional component in matrimony vine and the slag dregs of rice thereof |
| CN102886153A (en) * | 2012-10-24 | 2013-01-23 | 周学义 | Method for extracting eyesight improving functional components in Chinese wolfberries and dregs thereof |
| CN103149165A (en) * | 2013-01-28 | 2013-06-12 | 西北农林科技大学 | Orange cabbage carotenoid extracting and measuring method |
| CN103504435A (en) * | 2013-10-13 | 2014-01-15 | 全亚平 | Zeaxanthin-rich eyesight-improving wolfberry beverage and production method thereof |
| CN103504435B (en) * | 2013-10-13 | 2016-08-17 | 全亚平 | Wolfberry bright eye beverage and production method thereof rich in zeaxanthin |
| CN104803901A (en) * | 2014-01-27 | 2015-07-29 | 中国科学院大连化学物理研究所 | Method for preparing zeaxanthin through in situ enrichment |
| WO2015109657A1 (en) * | 2014-01-27 | 2015-07-30 | 中国科学院大连化学物理研究所 | Method for manufacturing nature zeaxanthin by means of in-situ concentration |
| CN106093264A (en) * | 2016-07-20 | 2016-11-09 | 福建省农业科学院作物研究所 | A kind of assay method of Fructus Fragariae Ananssae Xanthophyll Cycle Components |
| CN107141841A (en) * | 2017-07-04 | 2017-09-08 | 江苏食品药品职业技术学院 | A kind of wolfberry pigment product and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102040548A (en) | Method for extracting beta-carotene and zeaxanthin from Chinese wolfberry skin | |
| CN103450703B (en) | Method for preparing high-purity taste-removing purple sweet potato pigment | |
| CN110372554A (en) | A kind of industrial method quickly and efficiently extracting lutein and quercetagetin | |
| CN102690208A (en) | Method for extracting hydroxyl sanshool from zanthoxylum oil | |
| CN101768073A (en) | Method for preparing ferulic acid from Chinese angelica | |
| CN101870637B (en) | Technology for extracting and preparing policosanol | |
| CN103936643A (en) | Method for extraction and separation of xanthophyll and flavones in marigold | |
| CN108059628A (en) | A kind of fast preparation method of blueberry anthocyanin | |
| CN102850189B (en) | A kind of preparation method of high-purity saturation laccol and its formal derivatives | |
| CN102988605A (en) | Method for extracting lycium barbarum extract by supercritical CO2 | |
| CN102020544B (en) | Process for extracting chalcone type ingredients from ashitaba | |
| CN102772521B (en) | Method for extracting coffee polyphenols from coffee bean | |
| CN103694213B (en) | A kind of extraction and isolation preparation method of Lignans in Schisandra chinensis monomer | |
| CN101831198A (en) | Preparation method of capsanthin | |
| CN102329221B (en) | Method for preparing isostearic acid | |
| CN102614308B (en) | Method for extracting bioactivator in hot chili residue through subcritical water | |
| CN104099023B (en) | Pimaric acid type resin acid product and method for extracting pimaric acid type resin acid product from torreya grandis aril | |
| CN105646314A (en) | Method for one-step extraction and saponification of marigold lutein | |
| CN103045354A (en) | Method for extracting seabuckthorn fruit by supercritical CO2 | |
| CN105503981A (en) | Method for extracting and separating anthocyanin from red cabbage | |
| CN102796034B (en) | Method for preparing lutein crystal from marigold flowers | |
| CN113501752B (en) | Acid purification method of coenzyme Q10 | |
| CN103396461A (en) | Separation and purification method for secoisolariciresinol diglucoside | |
| CN101311148B (en) | Process for double-aqueous-phase extracting and refining persimmon lycopene | |
| CN102816098B (en) | Method for extraction of zeaxanthin from Tagetes erecta L. |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110504 |