CN102058898B - Powder with antibacterial and haemostatic effects and preparation method and applications thereof - Google Patents
Powder with antibacterial and haemostatic effects and preparation method and applications thereof Download PDFInfo
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- CN102058898B CN102058898B CN 201110006521 CN201110006521A CN102058898B CN 102058898 B CN102058898 B CN 102058898B CN 201110006521 CN201110006521 CN 201110006521 CN 201110006521 A CN201110006521 A CN 201110006521A CN 102058898 B CN102058898 B CN 102058898B
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Abstract
The invention provides powder with antibacterial and haemostatic effects and a preparation method and applications thereof. The powder with antibacterial and haemostatic effects comprises silver-carrying aquatic grass, medical acrylic resin and calcium bentonite, wherein silver-carrying aquatic grass is aquatic grass adsorbed with high-valence silver ions. The powder has the following benefits: (1) the powder has strong antibacterial effect; (2) the powder has long-lasting antibacterial effect; (3) the powder can rapidly absorb the water in the blood on the surface of wound, and promote accelerated coagulation of the blood on the surface of wound within a few seconds; and the powder does not agglomerate, which is favorable for dispersion and convenient in application; (4) the powder contains calcium ions which is helpful for wound healing; and (5) the powder has no irritation to human body.
Description
Technical field
The present invention relates to medicine and hygiene fields, relate in particular to a kind of sterilization haemostatic powder and its production and application.
Background technology
In the daily life, people usually run into and need sterilize and the hemostatic situation to traumatic surface or surgical wound surface.Wound-surface cover is generally the gauze class dressing that is formed by materials processings such as Cotton Gossypii, lint, non-woven fabrics or linen.But wound healing is slow when using these gauze class dressing, need often change dressings, and easily produces the wound bacterial infection, brings very big misery to the patient.
Publication number is that the Chinese patent of CN1123665A discloses a kind of antibacterial anti hemorrhagic dust granule made from the long-acting broad-spectrum antibacterial granule.This invention can directly be coated on wound surface, and is easy to use.But this antibacterial anti hemorrhagic dust granule has following deficiency: the silver that (1) is adsorbed on the Medulla Junci surface is non-valent microgranule silver, can only form the silver ion (Ag of lower valency when using in aqueous solution
+) go the sterilization, this monovalence silver ion because of more weak its sterilizing ability of oxidisability also a little less than; (2) raw material of Cai Yonging is a silver nitrate, does not remove harmful nitrate anion group in preparation process; (3) the product powder is used for patient's wound surface when hemostasis and easily forms agglomerate because of the moisture of absorption blood, is difficult to homodisperse and water absorption is few.
Summary of the invention
For addressing the above problem, the present invention aims to provide strong sterilization haemostatic powder of a kind of sterilizing ability and its production and application.This sterilization haemostatic powder can be used for preventing traumatic infection and effectively hemostasis, and is easy to use, is uniformly dispersed, and water absorption is big, and is non-stimulated to human body.
First aspect the invention provides a kind of sterilization haemostatic powder, forms by carrying silver-colored Medulla Junci, medical acrylic acid resin and calcium-base bentonite, and wherein carrying silver-colored Medulla Junci is the Medulla Junci that is adsorbed with high valence state silver ion.
The bactericidal property of silver ion gains public acceptance already, and has plurality of advantages such as odorlessness, nontoxic, non-stimulated, sterilization wide spectrum, anti-Drug resistance.Silver ion has different oxidisability and sterilizing ability with valence state is different: be higher than univalent silver ion (as, Ag
2+, Ag
3+) be high valence state silver ion, monovalence silver ion (Ag
+) be the lower valency silver ion, their oxidisability and the sterilizing ability (Ag that successively decreases in order
3+＞Ag
2+＞Ag
+＞Ag
0).This is because the oxidation-reduction potential of silver ion is high more, and easy more its surrounding space that makes produces elemental oxygen, and elemental oxygen has strong oxidizing property and can sterilize.Our result of the test has proved that also (conclusion page52) sees Table 1 to following two pieces of reports for 1. 2. Soap/Cosmetics/Chemical Specialties of Journal ofUEST ofChina Dec.2003vo1.36No6, March1994.
The sterilizing rate of table 1. different valence state silver ion
Can find out significantly that from table 1 valence state that the sterilizing rate of silver ion and they exist has substantial connection, along with valence state raises, its sterilizing rate also is to raise gradually.The sterilizing rate of the high valence state silver ion solution that the present invention uses is far above Ag
+Sterilizing rate 10.74%.
Therefore, sterilization haemostatic powder of the present invention uses high valence state silver ion, compares the sterilization haemostatic powder that contains the lower valency silver ion and has stronger oxidoreduction sterilizing ability.
Medulla Junci has microporous characteristics, can adsorb a large amount of silver ions.The Medulla Junci of having adsorbed a large amount of silver ions has abundant silver content, and long bactericidal action can be provided, and can be used for control and prevention wound surface bacterial infection, suppress the affected part inflammation.The length of Medulla Junci is not limit.Preferably, the length of Medulla Junci is 2～30mm.Also preferably, Medulla Junci is a nanoscale.
Be adsorbed with the preparation method of high valence state silver ion Medulla Junci: get silver peroxide (Ag
2O
2) and/or silver oxide (Ag
2O), put into reactor, add distilled water, stir after 15～60 minutes, dropwise add sulphuric acid, every stirring 10～60 minutes, the pH value of detection solution, make pH value to 2～3.5, clarified 2～10 hours, regulating the silver ion mass fraction is 0.01～1%, and the adding mass fraction is 0.3～10% hydrogen peroxide in reactor, stirred 1～2 hour, and made the mother solution that contains high valence state silver ion; Get Medulla Junci, the reactor that contains high valence state silver ion mother solution is housed, be stirred to Medulla Junci and all soak into the solution that contains high valence state silver ion, placed 2～10 hours, make and carry silver-colored Medulla Junci with putting into behind the sieve cloth parcel.
Preferably, the mass ratio of high valence state silver ion and Medulla Junci is 0.01～1: 1～2.
Carry after the silver-colored Medulla Junci drying and the medical acrylic acid mixed with resin.Preferably, the mass ratio that carries silver-colored Medulla Junci and medical acrylic acid resin is 1: 2～4.
The medical acrylic acid resin has high-hydroscopicity, and granule is thin, but the moisture in the fast Absorption wound surface blood, and conglomeration becomes gel in the several seconds, impels wound surface blood to accelerate to solidify.The medical acrylic acid resin that uses among the present invention can get the Mi Huagong company limited available from the Zhuhai City.Preferably, the medical acrylic acid resin is a fine-powdered.
Calcium-base bentonite has dilatancy, cementing properties and dispersibility, can help to absorb moisture and make it have the feature of disperseing not conglomeration, help carrying silver-colored Medulla Junci and fully contact wound surface, keep sterilization, prevent subinfection again, wherein calcium ion helps wound healing again.Smectite content height in the calcium-base bentonite.Montmorillonitum in China's the Tang Dynasty medical science masterpiece supplement to the Herbal is bentonite." Montmorillonitum is nontoxic, cures mainly medical herbs and all bacteriums, hot soup accent end clothes " also used bentonitic absorbability just and reached the antidotal effect.
Preferably, the mass ratio of calcium-base bentonite and medical acrylic acid resin is 1～3: 1.
Preferably, the smectite content height of calcium-base bentonite is 60～70%.
Preferably, calcium-base bentonite is Xinyang, Henan natural calcium base bentonite.The exchange capacity of its calcium ion is 53.43mmol/g, and water absorption rate is 296.94%, and far above other bentonite, avalanche becomes the shot shape rapidly, and wherein calcium ion can promote epithelization process, accelerating wound healing.
Also preferably, calcium-base bentonite can be nanoscale.More preferably, calcium-base bentonite is a nanoscale white calcium-base bentonite.
Second aspect the invention provides a kind of preparation method of sterilization haemostatic powder, may further comprise the steps:
(1) gets silver peroxide (Ag
2O
2) and/or silver oxide (Ag
2O), put into reactor, add distilled water, stir after 15～60 minutes, dropwise add sulphuric acid, every stirring 10～60 minutes, the pH value of detection solution, make pH value to 2～3.5, clarified 2～10 hours, regulating the silver ion mass fraction is 0.01～1%, and the adding mass fraction is 0.3～10% hydrogen peroxide in reactor, stirred 1～2 hour, and made the mother solution that contains high valence state silver ion;
(2) get Medulla Junci, the reactor that contains high valence state silver ion mother solution is housed, be stirred to Medulla Junci and all soak into the solution that contains high valence state silver ion, placed 2～10 hours, make and carry silver-colored Medulla Junci with putting into behind the sieve cloth parcel;
(3) will carry silver-colored Medulla Junci and take out from sieve cloth, and extract, oven dry makes the dry silver-colored Medulla Junci of carrying;
(4) get the dry silver-colored Medulla Junci of carrying, add medical acrylic acid resin and calcium-base bentonite, mix homogeneously, oven dry, pulverizing make sterilization haemostatic powder.
Wherein, make the mother solution that contains high valence state silver ion in the step (1).Proof procedure: get a high valence state silver ion mother solution for preparing as step (1), deliver to silver detects in City University of Hong Kong to the silver-colored solution of high price with the XPS method binding energy.Write " Ag3d in the examining report comment
5(366.3ev) value is lower than any Ag3d that has reported in the XPS handbook
5Value.Infer that very likely silver exists with high valence state " (KumarKaushik.V.Journal:J.Electron Spectrosc.Relat Phemon.56,273, (1991) .Ag is metallicform is～368.1ev, Ag in Ag
2O is～367.7ev, Ag in Ag
2O
2Is 367.3ev.).Can find out significantly that from the big report in city the silver-colored solution that uses among the present invention, its silver ion are to belong to high price silver, binding energy is 366.3ev, is lower than the binding energy (Ag of other valence state
0Binding energy be 368.1ev, Ag
+Binding energy be 367.7ev, Ag
2+Binding energy be 367.3ev, the high more binding energy of valence state of silver is just low more).
In the step (2), be to improve the performance of Medulla Junci absorption silver ion, preferably, Medulla Junci is earlier through 50～90% soak with ethanol, moistening and extract processing, reuse sieve cloth parcel.The length of Medulla Junci is not limit.Preferably, the length of Medulla Junci is prepared as 2～30mm.Also preferably, Medulla Junci is prepared as nanoscale.
The Medulla Junci raw material is light yellow, is transformed into white to brown after soaking into the solution that contains high valence state silver ion.
Along with Medulla Junci is soaked in the solution that contains high valence state silver ion gradually, the concentration of silver ions in the solution reduces gradually.In order to make Medulla Junci evenly to adsorb silver ion, preferably,, can further comprise and stirring 0.5～3 hour being stirred to after Medulla Junci all soaks into the solution that contains high valence state silver ion.Placed again subsequently 2～10 hours.
Step (3) is taken out from sieve cloth for carrying silver-colored Medulla Junci, extracts oven dry.Preferably, will carry silver-colored Medulla Junci and put into baking oven, under 50～120 ℃ of temperature, dry.
Step (4) is carried out compatibility for adding medical acrylic acid resin and calcium-base bentonite.
Preferably, the mass ratio that carries silver-colored Medulla Junci and medical acrylic acid resin is 1: 2～4.Medical acrylic acid resin of the present invention can get the Mi Huagong company limited available from the Zhuhai City.Preferably, the medical acrylic acid resin is selected fine-powdered medical acrylic acid resin for use.
Preferably, the mass ratio of calcium-base bentonite and medical acrylic acid resin is 1～3: 1.Preferably, to select smectite content for use be 60～70% calcium-base bentonite to calcium-base bentonite.Preferably, calcium-base bentonite is selected Xinyang, Henan natural calcium base bentonite for use.The exchange capacity of its calcium ion is 53.43mmol/g, and water absorption rate is 296.94%, and far above other bentonite, avalanche becomes the shot shape rapidly, and wherein calcium ion can promote epithelization process, accelerating wound healing again.Also preferably, calcium-base bentonite is selected nanoscale for use.More preferably, calcium-base bentonite is selected nanoscale white calcium-base bentonite for use.
Therefore the easy moisture absorption in put procedure because of medical acrylic acid resin and calcium-base bentonite raw material after carrying silver-colored Medulla Junci mix homogeneously with drying, needs oven dry.Preferably, bake out temperature is 50～80 ℃.
Pulverize after the oven dry and sieve.Preferably, pulverize the back and cross 200 mesh sieves, extracting screen underflow.
After making sterilization haemostatic powder, should further seal preservation.
In the preparation method of sterilization haemostatic powder of the present invention, related operation tool (comprising container) all can not react with silver ion.Reactor is preferably glass.Sieve cloth is preferably the Polyamide Yarns sieve cloth.Can use agitator in the whipping process, agitator is preferably nonmetal agitator.
The third aspect the invention provides a kind of application of sterilization haemostatic powder.The present invention can be used for postoperative wound surface bactericidal haemostatic also be can be used for the traumatic surface bactericidal haemostatic.
Sterilization haemostatic powder provided by the invention has following beneficial effect:
(1) sterilizing ability is strong, and high valence state silver ion has stronger redox, compares the sterilization haemostatic powder that contains the lower valency silver ion and has stronger sterilizing ability;
(2) sterilization is long-lasting, and the Medulla Junci that is adsorbed with a large amount of silver ions has abundant silver content, and long bactericidal action can be provided;
(3) high-hydroscopicity of medical acrylic acid resin and dilatancy, cementing properties and the dispersibility of calcium-base bentonite have been utilized, but the moisture in the fast Absorption wound surface blood, and in the several seconds, impel wound surface blood to accelerate to solidify, and not conglomeration, be beneficial to dispersion, easy to use;
(4) contain calcium ion, help wound healing;
(5) non-stimulated to human body.
The specific embodiment
The following stated is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also are considered as protection scope of the present invention.
Embodiment 1
A kind of preparation method of sterilization haemostatic powder may further comprise the steps:
(1) gets silver peroxide (Ag
2O
2), put into reactor, add distilled water, stir after 15 minutes, dropwise add sulphuric acid, every stirring 60 minutes, the pH value of detection solution, make pH value to 2, clarified 2 hours, regulating the silver ion mass fraction is 0.01%, and the adding mass fraction is 0.3% hydrogen peroxide in reactor, stirred 2 hours, and made the mother solution that contains high valence state silver ion;
(2) get the Medulla Junci that 1kg length is 2mm, the reactor that 100kg contains the mother solution of high valence state silver ion is housed, be stirred to Medulla Junci and all soak into the solution that contains high valence state silver ion, placed 10 hours, make and carry silver-colored Medulla Junci with putting into behind the sieve cloth parcel;
(3) will carry silver-colored Medulla Junci and from sieve cloth, take out, extract, put into baking oven, under 50 ℃ of temperature, dry, make the dry silver-colored Medulla Junci of carrying;
(4) get the dry silver-colored Medulla Junci of carrying, add medical acrylic acid resin and Xinyang, Henan natural calcium base bentonite.The dry mass ratio that carries silver-colored Medulla Junci, medical acrylic acid resin and calcium-base bentonite is 1: 2: 6, and mix homogeneously is crossed 200 mesh sieves in 50 ℃ of oven dry down, pulverizing back, and extracting screen underflow makes sterilization haemostatic powder, further sealing preservation.The medical acrylic acid resin gets the Mi Huagong company limited available from the Zhuhai City, is fine-powdered medical acrylic acid resin.Xinyang, Henan natural calcium base bentonite smectite content of selecting for use is 60%.
Embodiment 2
A kind of preparation method of sterilization haemostatic powder may further comprise the steps:
(1) gets silver oxide (Ag
2O), put into reactor, add distilled water, stir after 60 minutes, dropwise add sulphuric acid, every stirring 10 minutes, the pH value of detection solution, make pH value to 3.5, clarified 2 hours, regulating the silver ion mass fraction is 1%, and the adding mass fraction is 10% hydrogen peroxide in reactor, stirred 1 hour, and made the mother solution that contains high valence state silver ion;
(2) get the Medulla Junci that 2kg length is 30mm, the reactor that 100kg contains the mother solution of high valence state silver ion is housed, be stirred to Medulla Junci and all soak into the solution that contains high valence state silver ion, placed 2 hours, make and carry silver-colored Medulla Junci with putting into behind the sieve cloth parcel;
(3) will carry silver-colored Medulla Junci and from sieve cloth, take out, extract, put into baking oven, under 120 ℃ of temperature, dry, make the dry silver-colored Medulla Junci of carrying;
(4) get the dry silver-colored Medulla Junci of carrying, adding medical acrylic acid resin and smectite content are 70% calcium-base bentonite.The dry mass ratio that carries silver-colored Medulla Junci, medical acrylic acid resin and calcium-base bentonite is 1: 4: 4, and mix homogeneously is crossed 200 mesh sieves in 80 ℃ of oven dry down, pulverizing back, and extracting screen underflow makes sterilization haemostatic powder, further sealing preservation.The medical acrylic acid resin gets the Mi Huagong company limited available from the Zhuhai City, is fine-powdered medical acrylic acid resin.
Embodiment 3
A kind of preparation method of sterilization haemostatic powder may further comprise the steps:
(1) gets silver peroxide (Ag
2O
2), put into reactor, add distilled water, stir after 40 minutes, dropwise add sulphuric acid, every stirring 30 minutes, the pH value of detection solution, make pH value to 3, clarified 6 hours, regulating the silver ion mass fraction is 0.3%, and the adding mass fraction is 3% hydrogen peroxide in reactor, stirred 1.5 hours, and made the mother solution that contains high valence state silver ion;
(2) get the Medulla Junci that 2kg length is 10mm, earlier through 50% soak with ethanol, moistening and extract processing, put into behind the reuse sieve cloth parcel reactor that 100kg contains the mother solution of high valence state silver ion is housed, be stirred to Medulla Junci and all soak into the solution that contains high valence state silver ion, further stirred 0.5 hour, placed 8 hours, and made and carry silver-colored Medulla Junci;
(3) will carry silver-colored Medulla Junci and from sieve cloth, take out, extract, put into baking oven, under 70 ℃ of temperature, dry, make the dry silver-colored Medulla Junci of carrying;
(4) get the dry silver-colored Medulla Junci of carrying, adding medical acrylic acid resin and smectite content are Xinyang, Henan natural calcium base bentonite of 63%.The dry mass ratio that carries silver-colored Medulla Junci, medical acrylic acid resin and Xinyang, Henan natural calcium base bentonite is 1: 3: 6, and mix homogeneously is crossed 200 mesh sieves in 60 ℃ of oven dry down, pulverizing back, and extracting screen underflow makes sterilization haemostatic powder, further sealing preservation.The medical acrylic acid resin gets the Mi Huagong company limited available from the Zhuhai City, is fine-powdered medical acrylic acid resin.
Embodiment 4
A kind of preparation method of sterilization haemostatic powder may further comprise the steps:
(1) gets silver peroxide (Ag
2O
2), put into reactor, add distilled water, stir after 50 minutes, dropwise add sulphuric acid, every stirring 20 minutes, the pH value of detection solution, make pH value to 3.5, clarified 5 hours, regulating the silver ion mass fraction is 0.5%, and the adding mass fraction is 5% hydrogen peroxide in reactor, stirred 1.5 hours, and made the mother solution that contains high valence state silver ion;
(2) get the Medulla Junci that 2kg length is 10mm, earlier through 90% soak with ethanol, moistening and extract processing, put into behind the reuse sieve cloth parcel reactor that 100kg contains the mother solution of high valence state silver ion is housed, be stirred to Medulla Junci and all soak into the solution that contains high valence state silver ion, further stirred 3 hours, placed 6 hours, and made and carry silver-colored Medulla Junci;
(3) will carry silver-colored Medulla Junci and from sieve cloth, take out, extract, put into baking oven, under 65 ℃ of temperature, dry, make the dry silver-colored Medulla Junci of carrying;
(4) get the dry silver-colored Medulla Junci of carrying, adding medical acrylic acid resin and smectite content are Xinyang, Henan natural calcium base bentonite of 65%.The dry mass ratio that carries silver-colored Medulla Junci, medical acrylic acid resin and Xinyang, Henan natural calcium base bentonite is 2: 5: 6, and mix homogeneously is crossed 200 mesh sieves in 60 ℃ of oven dry down, pulverizing back, and extracting screen underflow makes sterilization haemostatic powder, further sealing preservation.The medical acrylic acid resin gets the Mi Huagong company limited available from the Zhuhai City, is fine-powdered medical acrylic acid resin.
Claims (2)
1. the preparation method of a sterilization haemostatic powder is characterized in that, may further comprise the steps:
(1) gets silver peroxide and/or silver oxide, put into reactor, add distilled water, stir after 15～60 minutes, dropwise add sulphuric acid, every stirring 10～60 minutes, the pH value of detection solution, make pH value to 2～3.5, clarified 2～10 hours, regulating the silver ion mass fraction is 0.01～1%, and the adding mass fraction is 0.3～10% hydrogen peroxide in reactor, stirred 1～2 hour, and made the mother solution that contains high valence state silver ion;
(2) get Medulla Junci, with putting into behind the sieve cloth parcel reactor that contains high valence state silver ion mother solution is housed, be stirred to Medulla Junci and all soak into the solution that contains high valence state silver ion, placed 2～10 hours, make and carry silver-colored Medulla Junci, described Medulla Junci is earlier through 50～90% soak with ethanol, moistening and extract processing, reuse sieve cloth parcel;
(3) will carry silver-colored Medulla Junci and take out from sieve cloth, and extract, oven dry makes exsiccant year silver-colored Medulla Junci;
(4) get the dry silver-colored Medulla Junci of carrying, add medical acrylic acid resin and calcium-base bentonite, mix homogeneously, oven dry, pulverizing make sterilization haemostatic powder;
Related operation tool all can not react with silver ion.
2. preparation method as claimed in claim 1 is characterized in that, bake out temperature is 50～120 ℃ described in the step (3).
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| CN 201110006521 CN102058898B (en) | 2011-01-13 | 2011-01-13 | Powder with antibacterial and haemostatic effects and preparation method and applications thereof |
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| CN102058898B true CN102058898B (en) | 2013-07-24 |
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| CN104874010A (en) * | 2015-05-28 | 2015-09-02 | 深圳市源兴纳米医药科技有限公司 | Composite zinc silver antibacterial agent contained chitosan fiber dressing and preparation method thereof |
| CN105030824B (en) * | 2015-08-20 | 2017-11-10 | 山东司邦得制药有限公司 | A kind of application of zinc-base montmorillonite and the sterile styptic powder of ca-montmorillonite |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1123665A (en) * | 1994-11-26 | 1996-06-05 | 蒋建华 | Long-effect and broad-spectrum antibiotic granules and its production |
| CN1214867A (en) * | 1997-10-21 | 1999-04-28 | 蒋华德 | Process for preparing bactericide containing silver |
| CN1772311A (en) * | 2004-11-09 | 2006-05-17 | 深圳市清华源兴生物医药科技有限公司 | Wound dressing containing Ag-Zn composition |
-
2011
- 2011-01-13 CN CN 201110006521 patent/CN102058898B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1123665A (en) * | 1994-11-26 | 1996-06-05 | 蒋建华 | Long-effect and broad-spectrum antibiotic granules and its production |
| CN1214867A (en) * | 1997-10-21 | 1999-04-28 | 蒋华德 | Process for preparing bactericide containing silver |
| CN1772311A (en) * | 2004-11-09 | 2006-05-17 | 深圳市清华源兴生物医药科技有限公司 | Wound dressing containing Ag-Zn composition |
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Address after: 518000 Guangdong city of Shenzhen province Nanshan District high tech Industrial Park, North Central Avenue, North Song Ping Road No. 1 Lite technology building south 10 layer 1001 Patentee after: Shenzhen Yuanxing pharmaceutical Limited by Share Ltd Address before: 518000, No. 19, Lang long road north, Nanshan District hi tech Development Zone, Guangdong, Shenzhen Patentee before: Shenzhen Yuanxing Nano-Pharmaceutical Co., Ltd. |