CN102266363A - Process for simultaneously extracting general flavone and total saponins from Chinese tamarisk twigs - Google Patents
Process for simultaneously extracting general flavone and total saponins from Chinese tamarisk twigs Download PDFInfo
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- CN102266363A CN102266363A CN2011102255603A CN201110225560A CN102266363A CN 102266363 A CN102266363 A CN 102266363A CN 2011102255603 A CN2011102255603 A CN 2011102255603A CN 201110225560 A CN201110225560 A CN 201110225560A CN 102266363 A CN102266363 A CN 102266363A
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Abstract
The invention belongs to the field of traditional Chinese medicines, and particularly relates to a process for simultaneously extracting general flavone and total saponins from Chinese tamarisk twigs. The process is characterized by comprising the following steps of: drying Chinese tamarisk twig serving as a raw material at a low temperature below 70 DEG C, smashing into coarse powder, performing hot reflux on the coarse powder with petroleum ether to remove oil-soluble substances such as chlorophyll and the like, volatizing and drying a solvent, adding a lower-alcohol organic solvent for extracting, filtering an extracting solution, recovering under reduced pressure, adding water into a concentrated solution to 0.5g crude medicament/ml, processing through combined macroporous absorption resin for saturated absorption, eluting with water, ammonia water, 20-50% ethanol and 60-80% ethanolin sequence, combining eluents of ammonia water and 20-50% ethanol, slowly adjusting the pH to 2-4, repeatedly washing precipitates with water, and drying to obtain the general flavone; adding medicinal active carbon into ethanol eluent of which the concentration is 60-80 percent, heating for refluxing, filtering in hot state, recovering ethanol from the filtrate under reduced pressure, concentrating and drying to obtain high-purity Chinese tamarisk twig total saponins of which the content is up to 80 percent. The process has the advantages of reasonable design, low cost and easiness for operation and mass production.
Description
Technical field
The invention belongs to the field of Chinese medicines, be specifically related to extract simultaneously the technology of total flavones and total saponins in the Cacumen Tamaricis.
Background technology
Cacumen Tamaricis be suspend Tamarix Ramulus et Folium Tamaricis (
Tamarix chinensisLour.) dry young browse.Sweet in the mouth, suffering, flat, GUIXIN, lung, stomach warp.Diffusing wind is arranged, induce sweat, the effect of rash.Ramulus et Folium Tamaricis secretes salt-secreting gland structure because of its unique biological, most plant have drought resisting, the characteristic of salt tolerant alkali, water-fast wet, impoverishment tolerant, China Tamarix seeds mainly are distributed in northwest drought, semiarid zone and coastal saline-alkali area, North China.The main component of Cacumen Tamaricis comprises flavonoid, triterpenes and volatile oil, have protect the liver, pharmacologically active such as antiinflammatory, antitumor, antipyretic-antalgic.Wherein triterpenoid compound comprises tamarixone, Ramulus et Folium Tamaricis alcohol, lupeol, β-amyrin, ursolic acid etc., have and protect the liver, antiinflammatory, antibiotic, anti-tumor activity, analgesic, analgesia, mice carried out the decoct of lumbar injection Cacumen Tamaricis, can obvious inhibitory action be arranged the mouse cough symptom due to the ammonia spraying.Facts have proved that Cacumen Tamaricis is also better to simple property senile chronic bronchitis effect, the type of panting takes second place, it is relatively poor to merge emphysema person.Zhao Runzhou etc. show that by experiment the Cacumen Tamaricis decoct all can obviously reduce the Mice Auricle capillary permeability when middle and high dosage, and the Mus ear chemical inflammation of antagonism due to the dimethylbenzene do not have the antiinflammatory effect in low dose group.Very significantly antiinflammatory action all appears in middle and high dosage group, and has shown certain dose-effect relationship.Analgesic experiment is the result show, the Cacumen Tamaricis decoct has obvious analgesic activity during by the 50g/kg gastric infusion, and the 1h effect is the most obvious after administration.And in, low dose group do not observe obvious analgesic activity.When the Cacumen Tamaricis decoct is pressed 7.5g/kg filling stomach in addition, the artificial fever rabbit also there is certain antipyretic effect.
At present, in the extracting method of the total flavones colleague report is arranged also in the Cacumen Tamaricis, adopt soak with ethanol extraction, methanol ultrasonic extraction more, obtain total flavones, these method gained flavone impurity are many, and content is low, and fail material effective component is fully extracted, raw material availability is low.
Summary of the invention
The purpose of this invention is to provide a kind of technology of extracting total flavones and total saponins in the Cacumen Tamaricis simultaneously, this method is simple to operate, be easy to industrialization.
The objective of the invention is to be achieved through the following technical solutions: with the raw material Cacumen Tamaricis in oven drying at low temperature below 70 ℃, be ground into coarse powder, coarse powder is removed liposoluble substances such as chlorophyll with petroleum ether (60-90 ℃) backflow 2-4h, with petroleum ether volatilize and drying after, add the low-carbon alcohols organic solvent extraction, extracting liquid filtering and reclaim under reduced pressure, concentrated solution adds water to 0.5g crude drug/ml, cross the saturated absorption of associating macroporous adsorbent resin, use earlier the deionized water eluting, discard water lotion, use ammonia more successively, 20%-50% ethanol, the 60%-80% ethanol elution merges ammonia and 20-50% ethanol elution, slowly regulate pH to 2-4, staticly settle, deionized water cyclic washing final vacuum drying gets total flavones; The 60-80% ethanol elution is added the medicinal carbon of 2%-5%, reflux, filtered while hot, decompression filtrate recycling ethanol concentrates, dry, the Cacumen Tamaricis total saponins.
Described low-carbon alcohols organic solvent is a kind of in ethanol, methanol, the isopropyl alcohol, and the liquid material is than being 6:1-12:1, and extracting method is a kind of in percolation, ultrasonic, Soxhlet, microwave or the reflux, extract.
Described associating macroporous adsorbent resin is two kinds of macroporous resins, be loaded on the position up and down of resin column respectively, the centre separates with absorbent cotton, upper strata and lower-layer resin ratio are 2:1, optional D101 of upper strata resin or AB-8 type macroporous adsorbent resin, a kind of among the optional DM301 of lower-layer resin, LD605, D140, D141, the HPD100.
Described ammonia is the ammonia spirit of 0.05-2%.
The invention has the beneficial effects as follows: the present invention only needed macroporous resin column one time, can obtain total flavones and total saponins in the Cacumen Tamaricis, by ammonia and low pure eluting, improve the flavone yield, to the total saponins processing of decolouring, improved the purity of saponin, the inventive method is reasonable in design, simple to operate, cost is low, is easy to industrialization production.
The specific embodiment
The present invention will the present invention is further illustrated in conjunction with specific embodiments, and following each embodiment only is used to illustrate the present invention, is not limitation of the present invention.
Embodiment 1:
Get Cacumen Tamaricis in oven drying at low temperature below 70 ℃, be ground into 20-60 order coarse powder, get the 1kg coarse powder and removed liposoluble substances such as chlorophyll in 2 hours with petroleum ether (60-90 ℃) reflux, extract,, with petroleum ether volatilize and drying after, add supersound extraction 1h in the 8L60% isopropyl alcohol supersound extraction jar, get extracting solution, extracting liquid filtering and reclaim under reduced pressure, concentrated solution adds water to 0.5g crude drug/ml and crosses the associating macroporous adsorptive resins, and this associating macroporous adsorbent resin is to separate with absorbent cotton in the middle of D101 macroporous resin and the DM301 macroporous resin, is loaded on the resin column the upper and lower respectively, the upper and lower resin ratio is 2:1, earlier use the deionized water eluting, discard water lotion, use 0.1% ammonia more successively, 30% ethanol, 60% ethanol elution, 0.1% ammonia and 30% ethanol elution are merged, transfer pH to 2.3, room temperature left standstill 20 hours, made the total flavones precipitation, filter, precipitate small amount of deionized water cyclic washing 5 times, vacuum drying obtains content and reaches 80% Cacumen Tamaricis total flavones; With the medicinal carbon of 60% eluent adding 3%, reflux, filtered while hot, decompression filtrate recycling ethanol, concentrated, vacuum drying obtain content and reach 70% Cacumen Tamaricis total saponins.
Embodiment 2:
Get Cacumen Tamaricis in oven drying at low temperature below 70 ℃, be ground into 20-60 order coarse powder, get the 1kg coarse powder and removed liposoluble substances such as chlorophyll in 3.5 hours with petroleum ether (60-90 ℃) reflux, extract,, with petroleum ether volatilize and drying after, add microwave extraction 1h in the 10L90% methanol microwave extraction tank, get extracting solution, extracting liquid filtering and reclaim under reduced pressure, concentrated solution adds water to 0.5g crude drug/ml and crosses the associating macroporous adsorptive resins, and this associating macroporous adsorbent resin is to separate with absorbent cotton in the middle of D101 macroporous resin and the D140 macroporous resin, is loaded on the resin column the upper and lower respectively, the upper and lower resin ratio is 2:1, earlier use the deionized water eluting, discard water lotion, use 0.05% ammonia more successively, 50% ethanol, 80% ethanol elution, 0.1% ammonia and 50% ethanol elution are merged, transfer pH to 3.5, room temperature left standstill 20 hours, made the total flavones precipitation, filter, precipitate small amount of deionized water cyclic washing 6 times, vacuum drying obtains content and reaches 75% Cacumen Tamaricis total flavones; With the medicinal carbon of 80% eluent adding 2.5%, reflux, filtered while hot, decompression filtrate recycling ethanol, concentrated, vacuum drying obtain content and reach 60% Cacumen Tamaricis total saponins.
Embodiment 3:
Get Cacumen Tamaricis in oven drying at low temperature below 70 ℃, be ground into 20-60 order coarse powder, get the 1kg coarse powder and removed liposoluble substances such as chlorophyll in 4 hours with petroleum ether (60-90 ℃) reflux, extract,, with petroleum ether volatilize and drying after, add microwave extraction 1h in the 12L75% ethanol microwave extraction tank, get extracting solution, extracting liquid filtering and reclaim under reduced pressure, concentrated solution adds water to 0.5g crude drug/ml and crosses the associating macroporous adsorptive resins, and this associating macroporous adsorbent resin is to separate with absorbent cotton in the middle of AB-8 macroporous resin and the LD605 macroporous resin, is loaded on the resin column the upper and lower respectively, the upper and lower resin ratio is 2:1, earlier use the deionized water eluting, discard water lotion, use 2% ammonia more successively, 25% ethanol, 70% ethanol elution, 0.1% ammonia and 25% ethanol elution are merged, transfer pH to 3.0, room temperature left standstill 20 hours, made the total flavones precipitation, filter, precipitate small amount of deionized water cyclic washing 6 times, vacuum drying obtains content and reaches 80% Cacumen Tamaricis total flavones; With the medicinal carbon of 70% eluent adding 4%, reflux, filtered while hot, decompression filtrate recycling ethanol, concentrated, vacuum drying obtain content and reach 70% Cacumen Tamaricis total saponins.
Embodiment 4:
Get Cacumen Tamaricis in oven drying at low temperature below 70 ℃, be ground into 20-60 order coarse powder, get the 1kg coarse powder and removed liposoluble substances such as chlorophyll in 2.5 hours with petroleum ether (60-90 ℃) reflux, extract,, with petroleum ether volatilize and drying after, add in the 6L65% isopropyl alcohol apparatus,Soxhlet's and extract 1h, get extracting solution, extracting liquid filtering and reclaim under reduced pressure, concentrated solution adds water to 0.5g crude drug/ml and crosses the associating macroporous adsorptive resins, and this associating macroporous adsorbent resin is to separate with absorbent cotton in the middle of D101 macroporous resin and the HPD100 macroporous resin, is loaded on the resin column the upper and lower respectively, the upper and lower resin ratio is 2:1, earlier use the deionized water eluting, discard water lotion, use 0.15% ammonia more successively, 20% ethanol, 60% ethanol elution, 0.1% ammonia and 20% ethanol elution are merged, transfer pH to 2.0, room temperature left standstill 20 hours, made the total flavones precipitation, filter, precipitate small amount of deionized water cyclic washing 5 times, vacuum drying obtains content and reaches 80% Cacumen Tamaricis total flavones; With the medicinal carbon of 60% eluent adding 5%, reflux, filtered while hot, decompression filtrate recycling ethanol, concentrated, vacuum drying obtain content and reach 70% Cacumen Tamaricis total saponins.
Embodiment 5:
Get Cacumen Tamaricis in oven drying at low temperature below 70 ℃, be ground into 20-60 order coarse powder, get the 1kg coarse powder and removed liposoluble substances such as chlorophyll in 3 hours with petroleum ether (60-90 ℃) reflux, extract,, with petroleum ether volatilize and drying after, add in the 7L60% ethanol Soxhlet extraction device and extract 1h, get extracting solution, extracting liquid filtering and reclaim under reduced pressure, concentrated solution adds water to 0.5g crude drug/ml and crosses the associating macroporous adsorptive resins, and this associating macroporous adsorbent resin is to separate with absorbent cotton in the middle of D101 macroporous resin and the LD605 macroporous resin, is loaded on the resin column the upper and lower respectively, the upper and lower resin ratio is 2:1, earlier use the deionized water eluting, discard water lotion, use 0.1% ammonia more successively, 30% ethanol, 75% ethanol elution, 0.1% ammonia and 30% ethanol elution are merged, transfer pH to 2.8, room temperature left standstill 20 hours, made the total flavones precipitation, filter, precipitate small amount of deionized water cyclic washing 4 times, vacuum drying obtains content and reaches 70% Cacumen Tamaricis total flavones; With the medicinal carbon of 75% eluent adding 3.5%, reflux, filtered while hot, decompression filtrate recycling ethanol, concentrated, vacuum drying obtain content and reach 65% Cacumen Tamaricis total saponins.
Embodiment 6:
Get Cacumen Tamaricis in oven drying at low temperature below 70 ℃, be ground into 20-60 order coarse powder, get the 1kg coarse powder and removed liposoluble substances such as chlorophyll in 2.5 hours with petroleum ether (60-90 ℃) reflux, extract,, with petroleum ether volatilize and drying after, add supersound extraction 1h in the 9L80% methanol supersound extraction jar, get extracting solution, extracting liquid filtering and reclaim under reduced pressure, concentrated solution adds water to 0.5g crude drug/ml and crosses the associating macroporous adsorptive resins, and this associating macroporous adsorbent resin is to separate with absorbent cotton in the middle of AB-8 macroporous resin and the D140 macroporous resin, is loaded on the resin column the upper and lower respectively, the upper and lower resin ratio is 2:1, earlier use the deionized water eluting, discard water lotion, use 0.05% ammonia more successively, 40% ethanol, 75% ethanol elution, 0.1% ammonia and 40% ethanol elution are merged, transfer pH to 3.4, room temperature left standstill 20 hours, made the total flavones precipitation, filter, precipitate small amount of deionized water cyclic washing 4 times, vacuum drying obtains content and reaches 80% Cacumen Tamaricis total flavones; With the medicinal carbon of 75% eluent adding 2%, reflux, filtered while hot, decompression filtrate recycling ethanol, concentrated, vacuum drying obtain content and reach 70% Cacumen Tamaricis total saponins.
Embodiment 7:
Get Cacumen Tamaricis in oven drying at low temperature below 70 ℃, be ground into 20-60 order coarse powder, get the 1kg coarse powder and removed liposoluble substances such as chlorophyll in 2 hours with petroleum ether (60-90 ℃) reflux, extract,, with petroleum ether volatilize and drying after, add supersound extraction 1h in the 11L70% ethanol ultrasonic extraction jar, get extracting solution, extracting liquid filtering and reclaim under reduced pressure, concentrated solution adds water to 0.5g crude drug/ml and crosses the associating macroporous adsorptive resins, and this associating macroporous adsorbent resin is to separate with absorbent cotton in the middle of AB-8 macroporous resin and the DM301 macroporous resin, is loaded on the resin column the upper and lower respectively, the upper and lower resin ratio is 2:1, earlier use the deionized water eluting, discard water lotion, use 0.2% ammonia more successively, 45% ethanol, 80% ethanol elution, 0.1% ammonia and 45% ethanol elution are merged, transfer pH to 4.0, room temperature left standstill 20 hours, made the total flavones precipitation, filter, precipitate small amount of deionized water cyclic washing 6 times, vacuum drying obtains content and reaches 70% Cacumen Tamaricis total flavones; With the medicinal carbon of 80% eluent adding 4.5%, reflux, filtered while hot, decompression filtrate recycling ethanol, concentrated, vacuum drying obtain content and reach 65% Cacumen Tamaricis total saponins.
Claims (4)
1. extract the technology of total flavones and total saponins in the Cacumen Tamaricis simultaneously, it is characterized in that: with the raw material Cacumen Tamaricis in oven drying at low temperature below 70 ℃, be ground into coarse powder, coarse powder is removed liposoluble substances such as chlorophyll with petroleum ether (60-90 ℃) backflow 2-4h, with petroleum ether volatilize and drying after, add the low-carbon alcohols organic solvent extraction, extracting liquid filtering and reclaim under reduced pressure, concentrated solution adds water to 0.5g crude drug/ml, cross the saturated absorption of associating macroporous adsorbent resin, use the deionized water eluting earlier, discard water lotion, use ammonia more successively, 20%-50% ethanol, the 60%-80% ethanol elution, ammonia and 20-50% ethanol elution are merged, slowly regulate pH to 2-4, staticly settle, deionized water cyclic washing final vacuum drying gets total flavones; The 60-80% ethanol elution is added the medicinal carbon of 2%-5%, reflux, filtered while hot, decompression filtrate recycling ethanol concentrates, dry, the Cacumen Tamaricis total saponins.
2. the technology of extracting total flavones and total saponins in the Cacumen Tamaricis simultaneously as claimed in claim 1, it is characterized in that: described low-carbon alcohols organic solvent is a kind of in ethanol, methanol, the isopropyl alcohol, the liquid material is than for 6:1-12:1, and extracting method is a kind of in percolation, ultrasonic, Soxhlet, microwave or the reflux, extract.
3. the technology of extracting total flavones and total saponins in the Cacumen Tamaricis simultaneously as claimed in claim 1, it is characterized in that: described associating macroporous adsorbent resin is two kinds of macroporous resins, be loaded on the position up and down of resin column respectively, the centre separates with absorbent cotton, upper strata and lower-layer resin ratio are 2:1, optional D101 of upper strata resin or AB-8 type macroporous adsorbent resin, a kind of among the optional DM301 of lower-layer resin, LD605, D140, D141, the HPD100.
4. the technology of extracting total flavones and total saponins in the Cacumen Tamaricis simultaneously as claimed in claim 1, it is characterized in that: described ammonia is the ammonia spirit of 0.05-2%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103599146A (en) * | 2013-11-11 | 2014-02-26 | 淮海工学院 | Preparation method and use of diuretic composition |
| CN104069063A (en) * | 2014-05-22 | 2014-10-01 | 安东 | Hydroxyfasudil pharmaceutical composition and preparation method thereof |
| CN105920065A (en) * | 2016-04-21 | 2016-09-07 | 肇庆医学高等专科学校 | Separation and purification method of begonia fimbritipula saponin and application of begonia fimbritipula saponin |
| CN109602770A (en) * | 2018-12-31 | 2019-04-12 | 山东省林业科学研究院 | A kind of Chinese tamarisk leaf leachate rapid extracting method |
-
2011
- 2011-08-08 CN CN2011102255603A patent/CN102266363A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103599146A (en) * | 2013-11-11 | 2014-02-26 | 淮海工学院 | Preparation method and use of diuretic composition |
| CN103599146B (en) * | 2013-11-11 | 2016-04-27 | 淮海工学院 | A kind of preparation method of diuretic compositions and purposes |
| CN104069063A (en) * | 2014-05-22 | 2014-10-01 | 安东 | Hydroxyfasudil pharmaceutical composition and preparation method thereof |
| CN104069063B (en) * | 2014-05-22 | 2019-03-26 | 西藏九瑞健康股份有限公司 | Fasudic hydrochloride pharmaceutical composition and preparation method thereof |
| CN105920065A (en) * | 2016-04-21 | 2016-09-07 | 肇庆医学高等专科学校 | Separation and purification method of begonia fimbritipula saponin and application of begonia fimbritipula saponin |
| CN109602770A (en) * | 2018-12-31 | 2019-04-12 | 山东省林业科学研究院 | A kind of Chinese tamarisk leaf leachate rapid extracting method |
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Application publication date: 20111207 |