CN102000111A - Preparation method of emergency survival hemostatic based on natural zeolite in Jinyun of Zhejiang - Google Patents
Preparation method of emergency survival hemostatic based on natural zeolite in Jinyun of Zhejiang Download PDFInfo
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Abstract
The invention discloses a preparation method of an emergency survival hemostatic based on natural zeolite in Jinyun of Zhejiang. The emergency survival hemostatic takes natural clinoptilolite and natural mordenite in Jinyun of Zhejiang Province as raw materials and comprises main components of monox, titanium oxide, alumina, ferric oxide, magnesia, calcium oxide, sodium oxide, potassium oxide and the like. The emergency survival hemostatic can be used for different medical occasions to stanch bleeding, can be used for preparing band aids, transfusion plasters, self-adhesion dressing, first-aid packets and the like by being mechanically combined with other medical materials and medical instruments. Meanwhile, bacteriophage, anodyne and the like can be adsorbed in the emergency survival hemostatic by using the ion exchange characteristic of the emergency survival hemostatic; the emergency survival hemostatic can be used as a medical transmission carrier; and other ions can be loaded by using the ion exchange characteristic of the emergency survival hemostatic, thereby better curative effect can be obtained. The emergency survival hemostatic based on natural zeolite in Jinyun of Zhejiang has the advantages of high stanching speed, low heat release, asepsis, apyrogeneity, non-cytotoxicity, no sensitivity response, harmlessness to skin, no reducing substances, no acid-base excitability and low cost, can extract content heavy metal with extremely-low content and is convenient for use.
Description
Technical field
The present invention relates to a kind of preparation method of emergency haemostatic, particularly a kind of preparation method that is used for the treatment of the hemorrhage Jinyun county, Zhejiang province natural zeolite hemorrhage of the uncontrollable mortality trunk of conventional hemostasis measure.
Background technology
Emergency haemostatic is an emerging research field in the world.Emergency haemostatic is primarily aimed at the outer damaging the spleen and stomach emergency that The blood streamed down and develops.(3 minutes) just can control the emergency as aorta is bled in a short period of time, for further medical treatment tries to gain time precious to one.
Ministry of Public Health statistics according to 2002 causes that wound and poisoning are number five in the ten big factors of people's death, and the number that therefore die every year is up to 9,500,000.Severe loss of blood is the biggest factor that causes died of wounds, and about 67% people dies from uncontrollable losing blood.Traumatogenic main cause mainly contains three: 1) war.In March, 2003～2008 year March, the war in Iraq causes 600,000 Irapi civilians and 4000 US soldier death.According to statistics, it is to die because of severe loss of blood before arriving at the medical center that the people who dies has half.Repeatedly the war casualty also discloses 30%～60% death according to statistics and comes from severe loss of blood.Treatment of war wound studies show that, if fell in battle so and percentage of died of wound will reduce greatly to obtain treatment in 1～3 hour by hemorrhage being effectively controlled after wound for the wounded, the treatment of war wound level will improve greatly.The emergency haemostatic at initial stage (as Quikclot) is mainly used in military, at using such as emergencies such as aorta are hemorrhage.The LSRHA material Quikclot of the Shi Yonging life of having saved up to a hundred US soldiers afield becomes the fight auxiliary equipment of the officers and men of marine corps of U.S. army indispensability.2) vehicle accident: this is the main cause of global youngster (being lower than 25 years old) and China common people unexpected death.World Health Organization (WHO) in 2007 report points out, has every year more than 400,000 the youngster less than 25 years old die from vehicle accident.The dead people more than 100,000 6 thousand of China's calendar year 2001 road traffic accident, account for national all kinds of death by accident total numbers of persons ~ 78%.China's road traffic accident fatality rate 10 years (1993-2002) meansigma methods of coming is up to 25.5% even more noteworthy, and the U.S. is 1.3%, and Japan is 0.9%, and Canada is 1.5%.The road traffic that a main cause that causes China's motor-vehicle accident fatality rate to remain high is China and the accident emergency lifesaving mechanism of vehicle itself are not built entirely.Back wounded body takes place in vehicle accident can not obtain treatment rapidly, so that many people are dead because of severe loss of blood.According to statistics, in most contingencies, the immediate cause that causes wounded body's death is not the injury that accident itself causes, but severe loss of blood.85% traffic death occurred in 30 minutes.At 30 minutes of this preciousness, the wounded if can obtain treatment, and the wound hemorrhage situation can be effectively controlled, and the vehicle accident fatality rate will descend greatly.3) major natural disasters.Can cause a large amount of casualties at short notice as natural disasters such as earthquake, tsunami and severe tropical storms.The 8.0 grades of violent earthquakes in Wenchuan, Sichuan on the 12nd in May in this year have caused 51151 people's death by 10 o'clock on the 22nd May, and 288431 people are injured.Rescue the wounded after the earthquake and divide six First aid procedures, be respectively hemostasis, fix, wrapping, ventilation, carrying and basic life support.Wherein hemostasis is a step at first, is the key of rescuing life.So far, domesticly be used for, the emergency haemostatic product of severe bleeding is few, hemorrhage commonly used has tourniquet, gauze and YUNNAN BAIYAO, they in, the quick-acting haemostatic powder effect of severe bleeding is limited.
Francis X.Hursey was not intended to find that zeolite molecular sieve has good anastalsis and applied for patent in 1989 the eighties in 20 century.At the beginning of 2002, Z-Medica company sets up, the novel hemostatic material of special Development and Production commodity Quikclot by name, this material is synthetic zeolite (the A type zeolite with 75%, the LTA structure) the composite type zeolite hemostatic material that mixes as binding agent for substrate and 25% clay, use at present zeolite molecular sieve material to obtain the drugs approved by FDA listing as the novel hemostatic material Quikclot of main body, no matter in laboratory (especially in the field operations battlefield) still in practice, its haemostatic effect and improve survival rate two aspects and all be better than traditional hemostatic material.People generally believe that its mechanism mainly is to rely on the superpower absorbability of molecular screen material at present, can in the several seconds, blot the moisture in the wound outflow blood, and do not absorb erythrocyte, platelet and other thrombins, thereby make thrombin concentrate and bring into play immediately anastalsis, simultaneously because Quikclot its surface in blood has negative charge, thereby excited the intrinsic coagulation passage, thus quicken coagulation process, reach the purpose of quick-acting haemostatic powder.Because Quikclot does not possess physics and chemism, thereby can not cause any anaphylaxis, can not cause wound infection yet, uses as safe as a house.The U.S. has all used Quikclot in Afghanistan and Irak military operation, it is very satisfied that effect is made us.The more important thing is that effect is much better than traditional hemostasia products because easy to use, Quikclot is entering average family, and its market prospect is very bright.
But Quikclot can bring bigger side effect to the wounded in coagulation process, mainly is because Quikclot can discharge a large amount of heats when contacting with blood, so that the muscular tissue of burning.Researcher finds that after by exchange silver ion heat obtains reduction by a relatively large margin, and antibacterial ability also significantly improves simultaneously, but but reduces significantly by the anthemorrhagic performance of Quikclot after the exchange silver ion.Therefore research worker has to seek other approach to reduce the heat effect of Quikclot.
Because the Jinyun county, Zhejiang province natural zeolite is the same with traditional molecular sieve, chance blood can absorb rapidly, swelling, not only can accomplish only to absorb moisture and do not absorb thrombin through effects such as physics, chemistry, biologies, reach the enrichment latter's purpose, thereby promote the thrombin activation and adhere to platelet, Jinyun county, Zhejiang province natural zeolite its surface in blood also has negative charge simultaneously, thereby excited the intrinsic coagulation passage, thereby the acceleration coagulation process promotes thrombosis, reaches the purpose of quick-acting haemostatic powder.Simultaneously have more superior character in some aspects, can become the research of novel hemostatic material to guarantee it.Jinyun county, Zhejiang province natural zeolite thermal discharge is few, nature content abundant because compare with Quikclot; The price of Quikclot is 150 yuan/bag (100 gram), and Jinyun Jinyun county, Zhejiang province natural zeolite ore is gone down the hill valency less than 0.02 yuan/100 grams, and tangible price advantage is arranged.And the ion-exchange capacity of Jinyun county, Zhejiang province natural zeolite is strong, by the exchange calcium ion can reinforcing material the blood coagulation performance.
Studies show that Jinyun county, Zhejiang province natural zeolite hemorrhage has characteristics such as anthemorrhagic speed is fast, aseptic, apyrogeneity, no cytotoxicity, no sensitivity response, no skin irritation, and easy to use, cost is low, has better market prospect.So far, do not see to have the Jinyun county, Zhejiang province natural zeolite is applied to blood coagulation material, treatment of wounds and outer wound reparation and Jinyun county, Zhejiang province natural zeolite and multi-form combinations such as medical bandage, medical adhesive, be used for the domestic and international patent document report that outer wound is repaired.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of novel Jinyun county, Zhejiang province natural zeolite hemorrhage.
The present invention proposes a kind of is the technology of feedstock production emergency haemostatic with the Jinyun county, Zhejiang province natural zeolite, selected raw material is the Jinyun county, Zhejiang province natural zeolite in the present invention's experiment, and described Jinyun county, Zhejiang province natural zeolite comprises Jinyun county, Zhejiang province natural mordenite or natural clinoptilolite or both mixture.The main component of Jinyun county, Zhejiang province natural zeolite is: silicon oxide, titanium oxide, aluminium oxide, ferrum oxide, magnesium oxide, calcium oxide, sodium oxide and potassium oxide etc.Wherein the total content of silicon oxide and aluminium oxide surpasses 70%.Be that the Jinyun county, Zhejiang province natural zeolite is ground into certain particle diameter by Chinese medicine grinder among the present invention, the present invention has simultaneously done corresponding improvement on the basis of Jinyun county, Zhejiang province natural zeolite, thereby obtain being rich in the modification Jinyun county, Zhejiang province natural zeolite of calcium ion, obtained having the zeolitic material of efficient hemostatic function.Therefore, can be used for different medical applications hemostasis, with other medical materials, medical apparatus and instruments combination, can be made into adhesive bandage, infusion patch, sticking dressing, tablet and capsule core material, operation bag, first-aid kit etc., utilize the adsorbable antibiotics of characteristics and the analgesic of its micropore to equal wherein simultaneously, can also be as drug delivery carrier; Utilize its ion exchange property can other ions of load, thereby obtain better therapeutic.Fast, the low heat release of Jinyun county, Zhejiang province natural zeolite hemorrhage anthemorrhagic speed of the present invention, aseptic, apyrogeneity, no cytotoxicity, no sensitivity response, no skin irritation, easy to use and cost is low.
Jinyun county, Zhejiang province natural zeolite emergence haemostatic preparation process is as follows:
(1) zeolite granulating:. block Jinyun county, Zhejiang province natural zeolite is ground into particles of different sizes by Chinese medicine grinder, obtains the Jinyun county, Zhejiang province natural zeolite granule of different-grain diameter (1 micron～1 millimeter) by screen;
(2) the Jinyun county, Zhejiang province natural zeolite after will pulverizing is by deionized water wash 3 times;
(3) the Jinyun county, Zhejiang province natural zeolite is carried out Ca ion exchange, obtain the Jinyun county, Zhejiang province natural zeolite after the Ca ion exchange;
(5) with the Jinyun county, Zhejiang province natural zeolite after the Ca ion exchange 200～500
oSterilization processing is 1～24 hour under the C temperature, obtains the aseptic Jinyun county, Zhejiang province natural zeolite emergence haemostatic after the modification.
Deionized water wash of the present invention is for 3 times that Jinyun county, Zhejiang province natural zeolite granule is mixed stirring with deionized water by the solid-to-liquid ratio of 1g/10ml, 10 min after-filtration, triplicate, the Jinyun county, Zhejiang province natural zeolite granule after obtaining washing.
Ca ion exchange of the present invention be with the washing after Jinyun county, Zhejiang province natural zeolite and concentration be the CaCl of 0.1～5.0mol/L
2Solution is pressed the solid-to-liquid ratio of 1g/20ml and is mixed, and room temperature reaction 24h uses deionized water wash three times, 120
oObtain the Jinyun county, Zhejiang province natural zeolite after the ion exchange after the C oven dry.
The present invention has following advantage:
1, operation is simple, and abundant raw material is cheap and easy to get, and it is convenient to use, and haemostatic effect is good, low heat release.
2, its suction heat that exothermic reaction produced of Jinyun county, Zhejiang province natural zeolite is therefore little to body hot injury side effect.
3, the Jinyun county, Zhejiang province natural zeolite is significantly improved through its anthemorrhagic performance after loading calcium ion.
4, the distinctive porous of Jinyun county, Zhejiang province natural zeolite, more adsorbable antibiotics or analgesic etc. help the treatment of wound.This material can mix use with multiple hemostatic material, if you would take off soil, Gypsum Fibrosum, Ophicalcitum etc.And can reduce the heat that the suction reaction produces to a certain extent, reduce clotting time simultaneously.This material can also be used for the hemostasis of different medical applications, with other medical materials, medical apparatus and instruments combination, can be made into adhesive bandage, infusion patch, sticking dressing, tablet and capsule core material, operation bag first-aid kit etc.; This material can also play slow release and controlled-release function as the additive of multiple medicinal tablet, powder.
5, but Jinyun county, Zhejiang province natural zeolite hemorrhage of the present invention has fast, the low heat release of anthemorrhagic speed, aseptic, apyrogeneity, no cytotoxicity, no sensitivity response, no skin irritation, no reducing substances, extremely low, the easy to use and low cost and other advantages of no soda acid zest extracting heavy metal.
Description of drawings
Fig. 1 is for natural clinoptilolite hemostatic material related among the present invention
XRDSpectrogram.
Fig. 2 is a natural mordenite tcrude ore involved in the present invention and respectively through 700 ℃ of roastings, 1mol/L NH
4The XRD figure spectrum of Cl ammoniumization, the acid-treated natural mordenite of 6mol/L HCl.
Fig. 3 is the sem photograph of Jinyun county, Zhejiang province natural clinoptilolite.
Fig. 4 is the sem photograph of Jinyun county, Zhejiang province natural mordenite.
Fig. 5 is the coagulation time test result of natural clinoptilolite, modenite hemostatic material and other hemostatic materials, wherein the blank group is the situation of hemostatic material of no use, matched group uses commercialization hemorrhage Quikclot and synthesizing flokite, and experimental group is the hemostatic material (error line is ± 0.16) with the exploitation of this experimental group.
Fig. 6 is the coagulogram (error line ± 0.15) of the natural clinoptilolite of washing, modification among the present invention.
The exothermic effect figure of the natural mordenite described in Fig. 7 the present invention, wherein Quikclot, fast-acting nemostatic powder are control material (error line is that three experimental results obtain).
Fig. 8 is the cytotoxicity figure (curve is obtained by the meansigma methods of 3 groups of data) of the lixiviating solution of natural clinoptilolite among the present invention.
The specific embodiment
The invention is further illustrated by the following examples.
The present invention selects the Jinyun county, Zhejiang province natural zeolite as raw material, and the XRD figure of Jinyun county, Zhejiang province natural clinoptilolite spectrum is seen accompanying drawing 1, and sem photograph is seen Fig. 3; XRD figure after the former powder of Jinyun natural mordenite and acid treatment, roasting, the ammoniumization is seen accompanying drawing 2, and sem photograph is seen accompanying drawing 4.
A certain amount of Jinyun natural zeolite is put into Chinese medicine grinder, about 5min of pulverizing time; The grain diameter that obtains after the pulverizing is at 1 micron～1 millimeter.With the dry 1h in 100 ℃ of baking ovens of the natural zeolite after the above-mentioned pulverizing.Its haemostatic effect and Quikclot are close, see accompanying drawing 5.
With sodium type natural zeolite and concentration behind the remodeling is the CaCl of 1.0mol/L
2Press the solid-to-liquid ratio of 1g/20ml and mix, room temperature reaction 24h does not have Ca with deionized water wash to solution
2+, and dry 24 h obtain the rich calcareous natural clinoptilolite of modification in 100 ℃ of baking ovens.Its haemostatic effect is seen accompanying drawing 6.
Get the 5.0g natural zeolite and mix stirring 1h, sucking filtration, washing then, 100 ℃ of dry 24h with a certain amount of water.Natural mordenite after obtaining washing, natural clinoptilolite, wherein water soluble ingredient reduces, and magnetisable material also reduces.Its haemostatic effect and Quikclot are close, see accompanying drawing 6.
At first at room temperature 1.90 g sodium hydroxide (NaOH) are dissolved in the 4 g deionized waters, stir, treat that NaOH dissolving back adds 1.43 g sodium aluminate (NaAlO
2), treat that sodium aluminate dissolving back adds 64.5 g deionized waters, stir 30min, add 9.82 g SiO at last
2, continue to stir 1 h.Mixed liquor is transferred in the water heating kettle at 170 ℃ of hydro-thermal 24 h, and filtration washing obtains synthetic modenite behind the dry 24h in 100 ℃ of baking ovens.Its haemostatic effect is seen accompanying drawing 5.
Get one of teat glass, add 10g natural zeolite of the present invention, and then add 10ml water, shake up, measure variations in temperature, the heat effect when reflecting the natural zeolite hemostasis by variations in temperature with thermometer.Its variations in temperature illustrates that much smaller than Quikclot and domestic commerce product fast-acting nemostatic powder the natural zeolite thermal discharge is considerably less, sees accompanying drawing 7.
Get an amount of natural zeolite of the present invention 100 ℃ of processing 1h in drying baker, take out a certain amount of pig whole blood (taking from Hangzhou meat processing combine) constant temperature in 25.00 ℃ of constant water bath box simultaneously, treat to begin the blood coagulation experiment behind the pig whole blood temperature stabilization; Get one in test tube, add 40 μ l CaCl
2Solution, and then add 100mg natural zeolite of the present invention adds 2ml pig whole blood at last, get rid of evenly with hands, picks up counting simultaneously, measures clotting time on the quiet blender of having proofreaied and correct rotating speed, angle in advance.
The natural clinoptilolite reducing substances is measured: with Jinyun county, Zhejiang province natural clinoptilolite and deionized water with 1/10 ratio lixiviate, get of the potassium permanganate solution titration of 10ml lixiviating solution then with 0.002mol/L, the potassium permanganate solution titration of 10ml deionized water with 0.002 mol/L, the poor≤0.5ml of potassium permanganate solution consumption are got in control experiment.
Natural clinoptilolite lixiviating solution pH measures: Jinyun county, Zhejiang province natural clinoptilolite and deionized water with 1/10 ratio lixiviate, are got 20ml lixiviating solution measurement pH then, and the pH value scope is 7.5 ± 0.5.
But the heavy metal element determination of lixiviate: Jinyun county, Zhejiang province natural clinoptilolite and deionized water with 1/10 ratio lixiviate, are got the 20ml lixiviating solution then and measured lixiviating solution, measure the content of metallic elements such as Pb, Cd, Ni in the lixiviating solution with ICP-AAS.The result is as shown in the table, the total metal content of surveying less than 1mg/L.
1. general toxicity test
Determination of test method according to ASTM F750-87 (2002), ASTM F619-03, ASTM F748-04 and GB/T16886.11 regulation.
The ICR mice (each ten of male and female, body weight 19-22g) that the attached first Ministry of Public Health combined multiple organs trans plantation of the hospital research emphasis laboratory animal laboratory of Zhejiang University is provided is divided into experimental group and each ten of matched groups (each five of male and female).With Jinyun county, Zhejiang province natural zeolite hemorrhage of the present invention with normal saline in 1:5 ratio lixiviate 3 days, lixiviating solution filters, and subsequently lixiviating solution is directly injected in the tested animal body, injects continuously three days, observe the weight of animals variation in 7 days, and compare with matched group (injecting normal saline).
The result shows that tested animal does not all have death.Animal does not have tangible abnormal response in half an hour, as tangible hair pine, jump etc.In seven days that observe continuously, all animals are good for and deposit, weight increase, and the weight increase no significant difference.As seen, Jinyun county, Zhejiang province natural zeolite hemorrhage avirulence of the present invention.
2. skin irritation test
Test according to regulation among the GB/T16886.10.
Experiment reagent: 3-5% formalin is used for positive control;
75% cotton ball soaked in alcohol;
Normal saline is used for negative control;
White vaseline.
Laboratory animal: the healthy adult rabbit, the attached first Ministry of Public Health combined multiple organs trans plantation of the hospital research emphasis laboratory animal laboratory of Zhejiang University provides.
Before the experiment, it is 4-6cm that area is respectively selected in back part of animal spinal column both sides
2The zone, remove by hair.With the ratio preparation of Jinyun county, Zhejiang province natural zeolite hemorrhage of the present invention and vaseline in 1:3, be evenly coated on the skin that rabbit exposes (about respectively select three), use the gauze of four layers of 4 * 4cm to cover immediately.Positive controls and negative control group are also each side selected three rabbit at spinal column, smear with 75% cotton ball soaked in alcohol earlier, behind the skin moisturizing 3ml 3-5% formalin or normal saline are spread upon on the skin of exposure, and the reuse gauze covers.The last left and right sides is all used nonirritant medical proof fabric and gauze to twine the rabbit back of the body and is fixed in three weeks of abdomen.Remove the covering gauze after 4 hours, clean covering part skin, and blot with gauze with 75% cotton ball soaked in alcohol.
According to the score standard (table 2) of following table, observed and recorded gauze position dermoreaction mark after removing gauze 24h, 48h, reaching 72h, and calculate PiI (PII) and the average PiI (APII) of every animal to material.
The table 2 dermoreaction standard of keeping the score
PiI (PII) be skin 24h, 48h, and the total points of 72h erythema edema divided by the value of the total gained of observing.
Average PiI (APII) is the summation of the PiI (PII) of all animals of experiment the value divided by the total gained of animal.
Reaction result is kept the score
Three groups of materials are all tested six times, respectively on rabbit vertebra each side three times.
The scoring of table 3 skin irritation test
Every animal is about 0 to the PiI (PII) of material
Average PiI (APII) is about 0
As seen Jinyun county, Zhejiang province natural zeolite hemorrhage of the present invention does not have the zest effect to skin.
3. cytotoxic effect
Cell line and culture medium: using cell is the IT3 cell, and experimental cell is the eugonic cell of 48h-72h.Culture medium is that DMEM adds 10%(V/V) hyclone.PH：7.2-7.4。
Experiment reagent:
The Jinyun county, Zhejiang province natural zeolite
Positive control: 0.6% phenol solution is dissolved in the DMEM culture medium that contains serum with phenol and makes.
Negative control: the fresh sterile DMEM culture medium that contains 10% hyclone.
5mg/ml MTT liquid.
Dimethyl sulfoxine (DMSO).
All reagent are aseptic condition.
The preparation of lixiviating solution: 1g Jinyun county, Zhejiang province natural zeolite of the present invention is added 10ml contain the fresh sterile DMEM cultivation of 10% hyclone based on 37 ℃ of lixiviate 24h.
Test is carried out on 1 96 orifice plate.The cell density of initial incubation liquid is about 50,000/ml, adds 200ul in every hole, makes that number of cells is about 8000～10000 in every hole.Each hole triplicate is in 5%(V/V) cultivate 24h in 37 ℃ of constant incubators of carbon dioxide air.
Discard former culture medium behind the 24h.Negative control group adds the fresh sterile DMEM culture medium that contains 10% hyclone of 200 ul, experimental group and positive controls add 20,40,60,120,160 respectively again, 200ul lixiviating solution and positive control solution, add negative controls again and make that liquor capacity is 200ul in every hole.Put into above-mentioned environment and cultivate 24h again.
Take out culture plate, discard the solution in the culture plate, every hole adds the MTT solution of 20ul, continues to cultivate 6h, inhales then and goes stock solution, adds the 150ul dimethyl sulfoxine, shakes ten minutes, and the 570nm wavelength is measured absorbance on immune microplate reader.(relative growth rate, RGR), and according to the form below carries out Cytotoxic evaluation of result to calculate the relative propagation degree of cell by following formula.
RGR%=experimental group mean light absorbency value/negative control group mean light absorbency value
Table 4
It is qualified that experimental result is 0 and 1 grade
Experimental result is 2 grades, should be in conjunction with cellular morphology analysis, overall merit.
Experimental result is defective for the 3-5 level.
The mtt assay experimental result is seen accompanying drawing 8.
By experimental result as can be known, the growth of the composition pair cell of Jinyun county, Zhejiang province natural zeolite hemorrhage of the present invention in the DMEM culture medium does not have the obvious suppression effect, therefore, and Jinyun county, Zhejiang province natural zeolite hemorrhage no cytotoxicity of the present invention effect.
4. thermal source experiment
According to second one of 200 years version of Pharmacopoeia of People's Republic of China, the endotoxin inspection technique is tested.
Get Jinyun county, Zhejiang province natural zeolite hemorrhage of the present invention and normal saline with the mixed of 1:5 in 37 ℃ of constant water bath box, be incubated one day.Get lixiviating solution.Be divided into three groups of positive controls, negative control, experimental group, add 0.1ml zeolite lixiviating solution in the experimental group, negative control group adds the 0.1ml normal saline, positive controls adds 0.1ml 0.1EU/ml endotoxin solution, add the 0.1ml tachypleus amebocyte lysate then, 37.5 constant temperature a period of time in ℃ water-bath, add developer constant temperature a period of time in 37.5 ℃ of water-baths more then.Add azo agents 1,2,3 then successively, measure absorbance or direct observation shade at last at the 545nm place.
The result shows the positive control composition brownish red that adds 0.1ml 0.1EU/ml, and negative control group and experimental group are all near colourless, and it is qualified that visible Jinyun county, Zhejiang province natural zeolite hemorrhage of the present invention detects through limulus reagent test, apyrogeneity.
Claims (3)
1. preparation method based on the Jinyun county, Zhejiang province natural zeolite emergence haemostatic, it is characterized in that: described Jinyun county, Zhejiang province natural zeolite emergence haemostatic is a raw material for choosing the Jinyun county, Zhejiang province natural zeolite, obtain hemorrhage through the modification processing and preparing, described Jinyun county, Zhejiang province natural zeolite comprises Jinyun county, Zhejiang province natural mordenite or natural clinoptilolite or both mixture, described Jinyun county, Zhejiang province natural zeolite is formed and is comprised: silicon oxide, titanium oxide, aluminium oxide, ferrum oxide, magnesium oxide, calcium oxide, sodium oxide and potassium oxide, wherein the total content of silicon oxide and aluminium oxide surpasses 70%; Its concrete preparation process is as follows:
(1) zeolite granulating:. block Jinyun county, Zhejiang province natural zeolite is ground into particles of different sizes by Chinese medicine grinder, obtains the Jinyun county, Zhejiang province natural zeolite granule of different-grain diameter (1 micron～1 millimeter) by screen;
(2) the Jinyun county, Zhejiang province natural zeolite after will pulverizing is by deionized water wash 3 times;
(3) the Jinyun county, Zhejiang province natural zeolite is carried out Ca ion exchange, obtain the Jinyun county, Zhejiang province natural zeolite after the Ca ion exchange;
(5) with the Jinyun county, Zhejiang province natural zeolite after the Ca ion exchange 200～500
oSterilization processing is 1～24 hour under the C temperature, obtains the aseptic Jinyun county, Zhejiang province natural zeolite emergence haemostatic after the modification.
2. want the preparation method of 1 described Jinyun county, Zhejiang province natural zeolite emergence haemostatic according to right, it is characterized in that described deionized water wash is for 3 times that Jinyun county, Zhejiang province natural zeolite granule is mixed stirring with deionized water by the solid-to-liquid ratio of 1g/10ml, 10 min after-filtration, triplicate, the Jinyun county, Zhejiang province natural zeolite granule after obtaining washing.
3. the preparation method of Jinyun county, Zhejiang province natural zeolite hemorrhage according to claim 1, it is characterized in that described Ca ion exchange be with the washing after Jinyun county, Zhejiang province natural zeolite and concentration be the CaCl of 0.1～5.0mol/L
2Solution is pressed the solid-to-liquid ratio of 1g/20ml and is mixed, and room temperature reaction 24h uses deionized water wash three times, 120
oObtain the Jinyun county, Zhejiang province natural zeolite after the ion exchange after the C oven dry.
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| CN112451734A (en) * | 2020-11-25 | 2021-03-09 | 联科华技术有限公司 | Application of monatomic catalyst as hemostatic agent |
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| CN101032516A (en) * | 2006-03-09 | 2007-09-12 | 青岛科技大学 | Preparing technique of zeolite type quick hemostasis agent |
| CN101357138A (en) * | 2008-07-29 | 2009-02-04 | 浙江大学 | Natural zeolite emergence haemostatic and preparation method thereof |
| CN101703519A (en) * | 2009-11-10 | 2010-05-12 | 浙江大学 | Method for improving hemostatic effect of external-use zeolite hemostat by calcium ion modification |
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- 2010-12-23 CN CN 201010550867 patent/CN102000111A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101032516A (en) * | 2006-03-09 | 2007-09-12 | 青岛科技大学 | Preparing technique of zeolite type quick hemostasis agent |
| CN101028284A (en) * | 2007-03-27 | 2007-09-05 | 中国人民解放军第四军医大学 | Externally-applied zeolite hemostat and its preparation |
| CN101357138A (en) * | 2008-07-29 | 2009-02-04 | 浙江大学 | Natural zeolite emergence haemostatic and preparation method thereof |
| CN101703519A (en) * | 2009-11-10 | 2010-05-12 | 浙江大学 | Method for improving hemostatic effect of external-use zeolite hemostat by calcium ion modification |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112451734A (en) * | 2020-11-25 | 2021-03-09 | 联科华技术有限公司 | Application of monatomic catalyst as hemostatic agent |
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