Summary of the invention
An object of the present invention is to provide a kind of new styptic sponge, this material good water absorption, safety, stable performance, it is low to have overcome in the prior art modified starch water-absorbent, shortcomings such as preparation instability.
Another object of the present invention is to provide the preparation method of described styptic sponge, the objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of styptic sponge is characterized in that: may further comprise the steps:
1) the modified starch raw material is carried out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change,
2) drying, freeze-drying under the low temperature obtains styptic sponge.
Preferably, the modified starch raw material in the step 1 is one or more the combination in pre-gelatinized starch, denaturated starch by acid, dextrin, Sumstar 190, esterification starch, etherification starch, cross-linking starch, graft starch, the composite modified starch.
Preferably, before step 1, among or add the radiation exposure treatment step afterwards.
Preferably, the wavelength of ray is 0.01nm-400 μ m.
Preferably, ray is X ray.
Preferably, ray is infrared rays or ultraviolet ray.
Preferably, gamma intensity is 0.8keV-1.5keV.
Preferably, radiation power is 400-600W.
Preferably, the x radiation x time is 8-12min.
Another technical scheme of the present invention designs the purposes of the styptic sponge for preparing by method of the present invention:
The hemostatic material that the blood surface of a wound is arranged for the preparation of people, Mammals, birds, Reptilia.
The blood surface of a wound is arranged or be used for hemostatic material under surgical operation, emergency care of trauma, laryngoscope, endoscope, the chamber mirror for the preparation of body surface, in-vivo tissue organ and body cavity inner tissue or organ.
For the preparation of the material that promotes organization healing.
Preferably, described tissue comprises sub-dermal soft tissue, muscle tissue, osseous tissue, cerebral tissue, nervous tissue, liver,kidney,spleen.
In the material that sticks together for the preparation of the tissue that prevents wound or organ and its hetero-organization on every side or organ.
The applicant finds that method of the present invention has following characteristics after having carried out a series of conditional filtering tests:
Beneficial effect of the present invention:
1. method of the present invention has no requirement to the kind of modified starch, the modified starch of seeing commonly used may be used to present method in the prior art, its water absorbent rate of the styptic sponge for preparing and rate of water absorption have tangible performance advantage all far above modified starch sponges of the prior art.For example compare with control group, water absorbent rate on average improves more than 35%, and rate of water absorption improves more than 1 times, and tangible performance advantage is arranged.
The radiation exposure step can be positioned at before the modified starch denaturation process, among or afterwards, as long as in the preparation whole process of modified starch, used the radiation exposure step, all can improve water absorbent rate and the rate of water absorption of the new modified starch of acquisition.
3. the kind of ray is very wide in range, and the ray of wavelength between 0.01nm-400 μ m all can be used for the present invention.
4. the present invention is by carrying out sex change again to existing modified starch, and in addition radiation exposure is handled, further broken up the structure of starch molecule, significantly improved its water absorbing properties, and selected preferred processing parameter by a large amount of testing sieves, make the styptic sponge for preparing be better than like product of the prior art at water absorbing properties, wide application prospect is arranged.Convenient, preparation more stable that styptic sponge of the present invention prepares, safety more benefits suitability for industrialized production.
Embodiment
Below in conjunction with embodiment the present invention is further described in detail, the embodiment that provides is only in order to illustrate the present invention, rather than in order to limit the scope of the invention.
Embodiment 1:
With the hydroxypropyl Staragel 90V through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, again this modified starch slurry is placed under the x-ray bombardment, irradiation 12min, X ray intensity is 0.8KeV, suction filtration is with alcohol washing, drying, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 1.
Embodiment 2:
Hydroxypropyl Staragel 90V slurry is placed under the x-ray bombardment, irradiation 12min, X ray intensity is 1.5KeV, suction filtration, with alcohol washing, drying, again through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 2.
Embodiment 3:
With hydroxyethylamyle through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, again this modified starch slurry is placed under the x-ray bombardment, irradiation 8min, X ray intensity is 0.8KeV, suction filtration is with alcohol washing, drying, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 3.
Embodiment 4:
The hydroxyethylamyle slurry is placed under the x-ray bombardment, irradiation 8min, X ray intensity is 1.5KeV, suction filtration, with alcohol washing, drying, again through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 4.
Embodiment 5:
With carboxymethyl starch through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, again this modified starch slurry is placed under the x-ray bombardment, irradiation 12min, X ray intensity is 1.5KeV, suction filtration is with alcohol washing, drying, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 5.
Embodiment 6:
The carboxymethyl starch slurry is placed under the x-ray bombardment, irradiation 8min, X ray intensity is 0.8KeV, suction filtration, with alcohol washing, drying, again through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 6.
Embodiment 7:
With cationic starch through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, again this modified starch slurry is placed under the uviolizing, irradiation 8min, irradiation power is 400W, suction filtration is with alcohol washing, drying, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 7.
Embodiment 8:
The cationic starch slurry is placed under the uviolizing, irradiation 12min, irradiation power is 600W, suction filtration, with alcohol washing, drying, again through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 8.
Embodiment 9:
With the hydroxypropyl Staragel 90V through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, again this modified starch slurry is placed under the uviolizing, irradiation 8min, irradiation power is 400W, suction filtration is with alcohol washing, drying, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 9.
Embodiment 10:
Hydroxypropyl Staragel 90V slurry is placed under the uviolizing, irradiation 8min, irradiation power is 600W, suction filtration, with alcohol washing, drying, again through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 10.
Embodiment 11:
With hydroxyethylamyle through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, again this modified starch slurry is placed under the uviolizing, irradiation 8min, irradiation power is 400W, suction filtration is with alcohol washing, drying, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 11.
Embodiment 12:
The hydroxyethylamyle slurry is placed under the infrared ray radiation, irradiation 8min, irradiation power is 400W, suction filtration, with alcohol washing, drying, again through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 12.
Embodiment 13:
With carboxymethyl starch through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, again this modified starch slurry is placed under the infrared ray radiation, irradiation 12min, irradiation power is 600W, suction filtration is with alcohol washing, drying, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 13.
Embodiment 14:
The carboxymethyl starch slurry is placed under the infrared ray radiation, irradiation 12min, irradiation power is 600W, suction filtration, with alcohol washing, drying, again through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 14.
Embodiment 15:
With cationic starch through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, again this modified starch slurry is placed under the infrared ray radiation, irradiation 12min, irradiation power is 400W, suction filtration is with alcohol washing, drying, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 15.
Embodiment 16:
The cationic starch slurry is placed under the infrared ray radiation, irradiation 2min, irradiation power is 400W, suction filtration, with alcohol washing, drying, again through chemical reagent such as propylene oxide, phosphoric acid carry out etherificate, crosslinked, esterification is repeatedly made new modified starch after the sex change, be lyophilize 15 hours under 15 handkerchiefs at-45 ℃, vacuum tightness, obtain styptic sponge 16.
Embodiment 17 control group experimental designs
Method according to the embodiment 1,3,4,5 of patent cn200710199682.3 prepares styptic sponge A respectively, C, D, E, group in contrast.
The water absorbent rate of embodiment 18 styptic sponges and the detection of rate of water absorption
Multiplying power that sponge sucks in water adopts centrifugal determination, is about to about 0.025g sponge as in the 2ml water, and balance 10min puts into whizzer then, under the 500rpm rotating speed, takes out after centrifugal 10 minutes, weighs and calculates the raffinate amount, and each sample test is removed mean value 6 times.
The rate of water absorption of sponge is observed by the German Dataphysics OCA40Micro of company video contact angle measurement.
Experimental result: the styptic sponge A that the 16 kinds of hemostasis starch that makes by embodiment 1-16 method and embodiment 17 control groups obtain, C, D, its water absorbent rate of E and rate of water absorption contrast are as shown in the table:
Table 2
Interpretation:
Can draw following conclusion by above experimental data:
1. method of the present invention has no requirement to the kind of modified starch, the modified starch of seeing commonly used may be used to present method in the prior art, its water absorbent rate of the styptic sponge for preparing and rate of water absorption have tangible performance advantage all far above modified starch sponges of the prior art.For example compare with control group, water absorbent rate on average improves more than 30%, and rate of water absorption improves more than 1 times, and tangible performance advantage is arranged.
The radiation exposure step can be positioned at before the modified starch denaturation process, among or afterwards, as long as in the preparation whole process of modified starch, used the radiation exposure step, all can improve water absorbent rate and the rate of water absorption of the new modified starch of acquisition.
3. the kind of ray is very wide in range, and the ray of wavelength between 0.01nm-400 μ m all can be used for the present invention.
Embodiment 4 modified starch styptic sponges are to the haemostatic effect of the hemorrhage model of liver
Test method:
Cut liver placenta percreta area 1.5cm * 2.5cm in the pig liver surface with scalpel, the surface of a wound degree of depth is 0.25cm, makes the hemorrhage surface of a wound, and the styptic sponge of employing has: styptic sponge 1-90, the styptic sponge that control group adopts has styptic sponge A, C, D, E.
Respectively the above-mentioned surface of a wound is stopped blooding.After hemorrhage, immediately styptic sponge is placed on the wound and also exerts pressure in sponge with medical surgical gloves or hemostatic gauze, blocking blood flow unclamps gloves or gauze behind 1~2min gently, observe haemostatic effect, gloves and gauze whether adhesion sponge and sludged blood, cause again hemorrhage when opening.Need not after the hemostasis modified starch sponges is taken away or removed, get final product but do suitable infiltration flushing with physiological saline.
Test-results:
Styptic sponge 1-16 haemostatic effect is fine, and easy to use.All styptic sponges are met and are sucked blood immediately behind blood and form the sponge-sludged blood colloid of viscosity with blood, all can control the hemorrhage of the liver surface of a wound effectively within 1 minute, and styptic sponge A, C, D, E just can control hemorrhage in the time more than 1.5 minutes.Styptic sponge 1-90 and liver wound tissue tight adhesion promote blood coagulation, and sludged blood does not stick together with the gauze dressing of pressing, and can not cause again hemorrhage.