CN103690956A - Hemostatic powder and preparation method thereof - Google Patents

Hemostatic powder and preparation method thereof Download PDF

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Publication number
CN103690956A
CN103690956A CN201310750493.6A CN201310750493A CN103690956A CN 103690956 A CN103690956 A CN 103690956A CN 201310750493 A CN201310750493 A CN 201310750493A CN 103690956 A CN103690956 A CN 103690956A
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China
Prior art keywords
chitosan
filtering residue
antarctic krill
preparation
styptic powder
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CN201310750493.6A
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Chinese (zh)
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赵晓丽
吴帅
黄卓瑶
潘浩波
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Shenzhen Institute of Advanced Technology of CAS
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Shenzhen Institute of Advanced Technology of CAS
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Priority to CN201310750493.6A priority Critical patent/CN103690956A/en
Publication of CN103690956A publication Critical patent/CN103690956A/en
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Abstract

The invention relates to the technical field of biological medicines, in particular to a preparation method of hemostatic powder. The preparation method comprises the following steps: uniformly mixing chitosan extracted from an antarctic krill shell with an antimicrobial medicine in a mass ratio of (2-4): 1, sterilizing at 120 DEG C, and packaging. The invention further provides components and contents of the hemostatic powder. The chitosan extracted from the antarctic krill shell as a raw material is used as a main component of the hemostatic powder; and compared with ordinary chitosan, the chitosan extracted from the antarctic krill shell has a better hemostatic effect because a chitosan source is small in pollution, chitosan quality is greatly optimized and a raw material with high degree of deacetylation can be extracted.

Description

A kind of styptic powder and preparation method thereof
Technical field
The present invention relates to biological medicine technology field, especially a kind of chitosan that utilizes is as styptic powder of one of composition and preparation method thereof.
Background technology
Hemorrhage is one of trauma patient cause of death.Bleeding control can obviously reduce its mortality rate quickly and efficiently.Simple surgical operation is Bleeding control completely, and the use of hemostatic material can greatly reduce amount of bleeding.At present, apply clinically more topical hemostatic agent and mainly contain powdery type (as zeolite, collagen powder and potato starch), mandruka class (gelfoam, collagen sponge), oxidized regenerated cellulose and Fibrin Glue (if speed is yarn), hemostatic gauze class etc.
Each own certain weak point of these hemostatic materials: gelatin collagen-based materials, from Corii Bovis seu Bubali, easily causes allergy due to species variation, increase the infection rate of wound, especially to the wound polluting, therefore application is restricted; Fibrin glue is derived from blood, may cause viral infection; Oxidized regenerated cellulose is loosely organized, and the poor adhesion to petechia has and causes hemorrhage possibility again, and bleeding stopping period is longer, poor to hemorrhage swift and violent person's effect, therefore be not suitable for applying and being restricted as wound hemostasis material separately; After porous zeolite and the potato starch moisture in absorbing blood, a large amount of heat be can emit, wound local necrosis, inflammatory reaction etc. caused.Some haemostatic effect of these hemostatic materials is imprecise, and some is expensive, and some uses inconvenient, all exists certain defective.
Chitosan has avirulence, nonirritant, good organization's compatibility, antibacterial, antiinflammatory, hemostasis, minimizing wound surface oozes out and promote wound tissue's regeneration, repair, the effect of healing, be easy to form gel and characteristic that can natural degradation, can be used as good hemostatic material.But the haemostatic effect of chitosan is relevant with its deacetylation, the very difficult medical chitosans that extract high-quality such as Crusta Penaeus seu Panulirus Carapax Eriocheir sinensis in general source, this has just affected the haemostatic effect of chitosan.
There is following shortcoming in existing chitosan styptic powder: raw material sources differ greatly, the raw material sources of existing chitosan are mainly from coastal waters Crusta Penaeus seu Panulirus Carapax Eriocheir sinensis, and the waters of coastal waters Crustacean life is subject to the phosphorous, nitrogenous of the direct discharge into sea in chemical plant and be subject to rain drop erosion to enter extra large pesticide and undressed Sewage Pollution containing waste water, the farmland of heavy metal, and health is caused to great harm.Existing chitosan is lower in quality, cannot meet the needs of high-quality medical chitosan.
Summary of the invention
For addressing the above problem, the invention provides the method that chitosan that a utilization extracts from Antarctic krill shell is made styptic powder, it comprises the steps:
By the chitosan extracting from Antarctic krill shell and antibacterials, according to mass ratio, be 2~4:1, evenly mix, at 120 ℃ of temperature, after sterilizing, encapsulate.
Wherein, described chitosan comprises the steps: from the extracting method of Antarctic krill
Step 1: get Antarctic krill shell and be submerged in strong base solution and boil 1 hour, be then washed to neutrality, obtain the first filtering residue after solid-liquid separation;
Step 2: described the first filtering residue is submerged in hydrochloric acid solution and is soaked under room temperature 1 hour, be then washed to neutrality, obtain the second filtering residue after solid-liquid separation;
Step 3: described the second filtering residue of take is reaction raw materials, repeating said steps one operation, obtains the 3rd filtering residue;
Step 4: described the 3rd filtering residue of take is reaction raw materials, repeating said steps two operations, obtain the 4th filtering residue; The 4th filtering residue described in vacuum drying;
Step 5: described the 4th filtering residue is submerged in strong base solution, and reflux is 1 hour at 110 ℃, is then washed to neutrality, then carries out solid-liquid separation;
Repeating said steps is inferior May Day, obtains rough chitosan; Rough chitosan described in vacuum drying;
Step 6: dried rough chitosan is dissolved to 1%(w/v) in acetum, form mixed system; Then the pH value that regulates described mixed system is 8.5, by after the solid product solid-liquid separation of separating out, then carries out lyophilization after washing, obtains product chitosan.
Wherein, in described step 1, the mass ratio of Antarctic krill shell and described highly basic is 5:3.
Wherein, in described step 1, the concentration of strong base solution is 1mol/L; In described step 2, the concentration of hydrochloric acid solution is 2mol/L.
Wherein, in described step 5, the mass concentration of strong base solution is 50%.
Wherein, described highly basic is NaOH or KOH.
Wherein, described antibacterials comprise one or more in nitrofuran compounds or nitro glyoxaline compound.
The present invention also provides this styptic powder, and it comprises chitosan and the antibacterials of extracting from Antarctic krill, and the mass ratio of described chitosan and antibacterials is 2:1~4:1.
Wherein, described antibacterials comprise one or more in nitrofuran compounds or nitro glyoxaline compound.
Beneficial effect:
The present invention uses Antarctic krill shell for the main component of raw material extraction chitosan as styptic powder, the chitosan extracting from Antarctic krill shell is compared with common chitosan aspect haemostatic effect, because the source of chitosan is of reduced contamination, in chitosan quality, there is larger optimization, can extract high deacetylized raw material, haemostatic effect is better.The antibacterial anti hemorrhagic powder that utilizes this chitosan to prepare, the effect that not only can play hemostasis can also also have antibacterial effect to wound.
The specific embodiment
To introduce in detail styptic powder of the present invention and preparation method thereof below.
The composition of this styptic powder is chitosan and the antibacterials of extracting from Antarctic krill, and its concrete preparation method is as follows:
First, from Antarctic krill, extract chitosan.
Step 1: get Antarctic krill shell 10g, add in the sodium hydroxide solution of 150ml, 1mol/L and boil 1 hour, be then washed to neutrality, obtain the first filtering residue after solid-liquid separation.
Step 2: described the first filtering residue is placed in to lower the immersion 1 hour of hydrochloric acid solution room temperature (23 ± 2 ℃) of 100ml, 2mol/L, is then washed to neutrality, obtain the second filtering residue after solid-liquid separation.
Step 3: the sodium hydroxide solution that described the second filtering residue is placed in to 100ml, 1mol/L boils 1 hour, is then washed to neutrality, obtains the 3rd filtering residue after solid-liquid separation.
Step 4: described the 3rd filtering residue is placed under 100ml, 2mol/L hydrochloric acid solution room temperature and is soaked 1 hour, be then washed to neutrality, obtain the 4th filtering residue after solid-liquid separation, the 4th filtering residue described in vacuum drying
Step 5: in the NaOH concentrated solution that is 50% by described the 4th filtering residue mass fraction, reflux takes off acetyl operation for 1 hour at 110 ℃, is then washed to neutrality, then carries out solid-liquid separation.
The de-acetyl operation of repeating step five once, obtains rough chitosan.Then rough chitosan described in vacuum drying.
Step 6: it is 1%(w/v that the rough chitosan after vacuum drying is dissolved in to quality-volume fraction) in acetum, form mixed system; Then adopting the NaOH solution of 0.1mol/L to regulate the pH value of described mixed system is 8.5.Now chitosan is separated out from mixed system, after filtering, obtains refining chitosan, carries out lyophilization after washing, obtains the product chitosan of brilliant white.
Then, adopt the above-mentioned chitosan extracting from Antarctic krill shell to prepare styptic powder.
For example, by the chitosan extracting from Antarctic krill shell and antibacterials (vancomycin), according to mass ratio, be 2:1~4:1, evenly mix, make the uniform particle diameter of styptic powder; Then at 120 ℃ of temperature, after sterilizing, encapsulate.
The antibacterials that the present embodiment adopts can be for example one or more in nitrofuran compounds or nitro glyoxaline compound.Specifically can be such as being the antibiotic such as furazolidone, furaltadone, nitrofurantoin, nitrofural or metronidazole, tinidazole.
For further illustrating the present invention, from the chitosan of Antarctic krill acquisition, have more excellent styptic activity, carry out following contrast experiment, concrete operations are as follows:
The chitosan extracting from Antarctic krill shell and sigma chitosan are done to mice docking haemostatic effect contrast experiment:
1. take chitosan powder (numbering 1) and 0.1gsigma chitosan powder (numbering 2) that 0.1g extracts from Antarctic krill shell, be placed in respectively two 2ml and show bottle 1 and show bottle 2, sterilizing is standby;
2. get the C57BL/6 mice of two same batch, weigh, amount tail is long;
3. with operation cut off mouse tail long 1/3rd after, the wound that will dock immediately inserts respectively to be shown bottle 1 and shows in bottle 2 while timing.Mice amount of bleeding when calculating blood flow stops.
Carry out respectively three groups of parallel laboratory tests, obtain average bleeding, refer to table 1.The haemostatic effect of the chitosan extracting from Antarctic krill shell is as can be seen from Table 1 better than sigma chitosan.This may be because Antarctic krill is a kind of abyssopelagic organism resource, the waters of life be not subject to heavy metal (such as, arsenic, lead, hydrargyrum, nickel and silver ion etc.) pollute, in its krill Crusta Penaeus seu Panulirus and body all containing harmful element.The Antarctic krill of take has optimized the quality of chitosan as raw material from source, thereby can prepare high deacetylized high-quality chitosan, usings this chitosan as the main component of styptic powder, can effectively improve the haemostatic effect of styptic powder.
The chitosan that table 1 extracts from Antarctic krill shell and the contrast of sigma chitosan haemostatic effect
Sample 1 2
Mice weight 23.5±0.5g 24.0±0.3g
Mouse tail is long 8.0±0.3cm 8.0±0.2cm
Docking length 3.0±0.5cm 3.0±0.3cm
Bleeding time <5min <5min
Dry weight 0.1g 0.1g
Weight in wet base 0.1281g±0.023g 0.1364±0.015g
Amount of bleeding 0.0281±0.023g 0.0364±0.015g

Claims (9)

1. a manufacture method for styptic powder, it comprises the steps:
By the chitosan extracting from Antarctic krill shell and antibacterials, according to mass ratio, be 2~4:1, evenly mix, at 120 ℃ of temperature, after sterilizing, encapsulate.
2. manufacture method according to claim 1, is characterized in that, described chitosan comprises the steps: from the extracting method of Antarctic krill
Step 1: get Antarctic krill shell and be submerged in strong base solution and boil 1 hour, be then washed to neutrality, obtain the first filtering residue after solid-liquid separation;
Step 2: described the first filtering residue is submerged in hydrochloric acid solution and is soaked under room temperature 1 hour, be then washed to neutrality, obtain the second filtering residue after solid-liquid separation;
Step 3: described the second filtering residue of take is reaction raw materials, repeating said steps one operation, obtains the 3rd filtering residue;
Step 4: described the 3rd filtering residue of take is reaction raw materials, repeating said steps two operations, obtain the 4th filtering residue; The 4th filtering residue described in vacuum drying;
Step 5: described the 4th filtering residue is submerged in strong base solution, and reflux is 1 hour at 110 ℃, is then washed to neutrality, then carries out solid-liquid separation;
Repeating said steps is inferior May Day, obtains rough chitosan; Rough chitosan described in vacuum drying;
Step 6: dried rough chitosan is dissolved to 1%(w/v) in acetum, form mixed system; Then the pH value that regulates described mixed system is 8.5, by after the solid product solid-liquid separation of separating out, then carries out lyophilization after washing, obtains product chitosan.
3. the preparation method of styptic powder according to claim 2, is characterized in that, in described step 1, the mass ratio of Antarctic krill shell and described highly basic is 5:3.
4. the preparation method of styptic powder according to claim 2, is characterized in that, in described step 1, the concentration of strong base solution is 1mol/L; In described step 2, the concentration of hydrochloric acid solution is 2mol/L.
5. the preparation method of styptic powder according to claim 2, is characterized in that, in described step 5, the mass concentration of strong base solution is 50%.
6. according to the preparation method of styptic powder described in claim 2~4 any one, it is characterized in that, described highly basic is NaOH or KOH.
7. the preparation method of styptic powder according to claim 1, is characterized in that, described antibacterials comprise one or more in nitrofuran compounds or nitro glyoxaline compound.
8. a styptic powder, is characterized in that, comprises chitosan and the antibacterials from Antarctic krill, extracted, and the mass ratio of described chitosan and antibacterials is 2~4:1.
9. styptic powder according to claim 7, is characterized in that, described antibacterials comprise one or more in nitrofuran compounds or nitro glyoxaline compound.
CN201310750493.6A 2013-12-31 2013-12-31 Hemostatic powder and preparation method thereof Pending CN103690956A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104758296A (en) * 2015-03-10 2015-07-08 江苏卓见医疗用品有限公司 Chitosan composite material containing novel active molecule, preparation method and application thereof
CN108743701A (en) * 2018-06-09 2018-11-06 江苏海尔滋生物科技有限公司 GSE- nitrofurazone flushing liquors and preparation method thereof
CN109602942A (en) * 2018-12-13 2019-04-12 青岛海汇生物工程有限公司 A kind of hemostasis of chitin, pain-relieving cotton preparation method

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JPH09249541A (en) * 1996-03-15 1997-09-22 Fudo Kosan:Kk Dentifrice
KR20000045851A (en) * 1998-12-30 2000-07-25 조정래 Preparation method for chitosan derivatives
CN1283634A (en) * 2000-08-28 2001-02-14 李高霖 Process for preparing water-soluble shitosan
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CN101974104A (en) * 2010-11-09 2011-02-16 厦门大学 Preparation method of chitosan

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09249541A (en) * 1996-03-15 1997-09-22 Fudo Kosan:Kk Dentifrice
KR20000045851A (en) * 1998-12-30 2000-07-25 조정래 Preparation method for chitosan derivatives
CN1283634A (en) * 2000-08-28 2001-02-14 李高霖 Process for preparing water-soluble shitosan
CN101200505A (en) * 2007-11-29 2008-06-18 湖北东方天琪生物工程股份有限公司 Method for preparing high deacetylate degree and high viscosity chitosan by using shrimp shell
CN101974104A (en) * 2010-11-09 2011-02-16 厦门大学 Preparation method of chitosan

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104758296A (en) * 2015-03-10 2015-07-08 江苏卓见医疗用品有限公司 Chitosan composite material containing novel active molecule, preparation method and application thereof
CN108743701A (en) * 2018-06-09 2018-11-06 江苏海尔滋生物科技有限公司 GSE- nitrofurazone flushing liquors and preparation method thereof
CN109602942A (en) * 2018-12-13 2019-04-12 青岛海汇生物工程有限公司 A kind of hemostasis of chitin, pain-relieving cotton preparation method

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Application publication date: 20140402