CN107213806B - A kind of filter membrane for filtrating leukocytes and preparation method thereof - Google Patents

A kind of filter membrane for filtrating leukocytes and preparation method thereof Download PDF

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CN107213806B
CN107213806B CN201710571716.0A CN201710571716A CN107213806B CN 107213806 B CN107213806 B CN 107213806B CN 201710571716 A CN201710571716 A CN 201710571716A CN 107213806 B CN107213806 B CN 107213806B
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filter membrane
sodium
filter
parts
filtrating leukocytes
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CN107213806A (en
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王衡东
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Guangzhou Economy Medical Science And Technology Co Ltd
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Guangzhou Economy Medical Science And Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06Organic material
    • B01D71/74Natural macromolecular material or derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61MDEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
    • A61M1/00Suction or pumping devices for medical purposes; Devices for carrying-off, for treatment of, or for carrying-over, body-liquids; Drainage systems
    • A61M1/34Filtering material out of the blood by passing it through a membrane, i.e. hemofiltration or diafiltration
    • A61M1/3496Plasmapheresis; Leucopheresis; Lymphopheresis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0079Manufacture of membranes comprising organic and inorganic components
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00Compounds of zinc
    • C01G9/02Oxides; Hydroxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08HDERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H6/00Macromolecular compounds derived from lignin, e.g. tannins, humic acids
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer

Abstract

The invention belongs to leukoreduction filter technical field, and in particular to a kind of filter membrane for filtrating leukocytes and preparation method thereof.Mainly it is made up of provided by the present invention for the filter membrane of filtrating leukocytes sodium alginate, nano zine oxide, chitosan oligosaccharide and amido sodium lignin sulfonate.The filter membrane for filtrating leukocytes that the present invention is prepared has adhesion by force and the advantages of stability is high, and material on filter membrane can be avoided to wash out or come off in use, effectively can be polluted anti-Hemostatic Oral Liquid;Simultaneously, have leucocyte and blood platelet filtration rate high provided by the present invention for the filter membrane of filtrating leukocytes, there is alleviation or anti-Hemostatic Oral Liquid cold agglutination phenomenon occurs during blood filtration, dredge the effect that filter sizes block, the filter quality of blood leucocyte can be ensured, the service life length of leukocyte filter membranes can also be extended, be a kind of ideal leukoreduction filter film.

Description

A kind of filter membrane for filtrating leukocytes and preparation method thereof
Technical field
The invention belongs to leukoreduction filter technical field, and in particular to a kind of filter membrane and its preparation for filtrating leukocytes Method.
Background technology
In medical procedure of transfusing blood, a variety of transfusion adverse effects can usually occur, its root is whole blood of the input containing leucocyte Or blood constituent can cause nonhemolytic febrific reaction, HLA isoimmunization, blood transfusion correlated virus infection and it is defeated The Adverse transfusion reaction such as graft versus host disease(GVH disease) after blood.Therefore, filtered out before blood transfusion the leucocyte in Blood Preparations have it is important Meaning.Leucocyte filter is the important method of filtrating leukocytes, and its principle is cut using the principle of machinery retardance and absorption Cell is left white, and allows the red blood cell that surface is smooth, deformability is stronger to pass through.At present, the requirement of the 3rd generation leucocyte filter is Rejection rate reaches 99.99%.
In addition, modern study shows that blood platelet can also induce body to produce antiplatelet antibody, antiplatelet antibody is one Kind autoantibody, the histoorgan nonrecognition to itself, can attack the histoorgan of itself, so as to cause damage.Therefore, in order to The side effect caused by platelet transfusion is reduced, people are directed to research one kind and also can expeditiously removed while except leucocyte-removing Remove hematoblastic filter membrane.There is correlative study to attempt the fibre diameter by reducing filter medium or aperture or increase filtering Jie in the past The packed density of matter removes the means of leucocyte-removing and blood platelet ability as filter medium is improved simultaneously.But apply the above method There can be hemofiltration process time lengthening and may result in erythrocyte membrane rupture and haemolysis occur.
At present, leukocyte filter membranes are changed using surface grafting or coating hydrophilic polymer to filtering material surface more Property, increase the wetability of filtering material, reduce the surface energy of filtering material surface and blood, increase filtering material contact blood Effective surface area, so as to increase the chance for catching leucocyte.But the hydrophily on filtering material surface is higher, blood platelet is more difficult to Activation, it can be easy to form water layer in material surface additionally by hydrogen bond of water and material etc., have and suppress plasma protein suction It is attached, especially fibrinous absorption, so as to reduce hematoblastic adhesiveness, hematoblastic retention is reduced.In addition, hydrophily The water solubility of polymer is stronger, dissolution in blood can be present.
Patent document CN103415309B discloses a kind of for removing material from blood or from blood derivatives Improved filter and method for obtaining the filter.Described filter includes the filter elements for accommodating stratiform The housing of part, layered filter cell include multiple layers, and at least one layer of layered filter cell is coated with Polyurethane, the molecular weight of the polyurethane are 12,000 dalton to 18,000 dalton, and are coated with the non-of polyurethane and knit The divine force that created the universe is mixed in the stratiform filter element formed in the less weaven goods of hydrophily, described stratiform filter element to leucocyte and Blood platelet, which is respectively provided with, preferably filters out effect.
Patent document CN106117580A discloses a kind of filter membrane modifying agent and its method of modifying for filtrating leukocytes, The filter membrane modifying agent modifies fibroin albumen, polyvinylpyrrolidone and acrylate copolymer with (0.052) by amidatioon: (0.2~1):1 mass ratio composition.Wherein, acrylate copolymer is by methyl methacrylate monomer and methacrylic acid two Methylamino acetate monomer is formed.The filter membrane modifying agent being prepared, which is dissolved in polar solvent such as water, is configured to solution, with infiltration Modified mode is coated processing to filter membrane, and the filter membrane after filter membrane modifier treatment has preferably wetting Property, stability and compatibility, higher rejection rate is respectively provided with to leucocyte and blood platelet, and wash out with relatively low modifying agent Rate, leachable is avoided to pollute.
However, current leukocyte filter membranes only focus on the design of cell rate filtering, tended to out during use Existing filter membrane is blocked the defects of causing service life relatively low or influence cell filtration quality, meanwhile, during filtering easily There is the pollution of blood, cause to bring bacterium inside receptor into, larger threat be present to the health of receptor.
The content of the invention
In order to overcome the defects of leukocyte filter membranes are present in the prior art.It is used to filter it is an object of the invention to provide one kind Filter membrane except leucocyte and preparation method thereof, to solve drawbacks described above.
The invention provides a kind of filter membrane for filtrating leukocytes, comprise the following steps:
100~200 parts of sodium alginate, 35~45 parts of nano zine oxide, 15~25 parts of chitosan oligosaccharide and amido lignin sulfonic acid 10~20 parts of sodium.
Further, the filter membrane for filtrating leukocytes includes following preparing raw material and its parts by weight:
15 parts of 160 parts of sodium alginate, 38 parts of nano zine oxide, 22 parts of chitosan oligosaccharide and amido sodium lignin sulfonate.
Further, the preparation method of the nano zine oxide is:
A. weigh zinc nitrate to add in deionized water, stir to being completely dissolved, be subsequently added into sodium carbonate, stirring is to having reacted Entirely, centrifuge, obtain white depositions;
B. lauryl glucosyl is added toward the obtained white depositions of step a, stirs 5~8min, be subsequently added into three TRIM, 10~20min is stirred, obtains mixed liquor;
C. the obtained mixed liquors of step b being heated to 130~140 DEG C, insulation stands 30~40min, is then passed through nitrogen, Continue to be heated to 250~300 DEG C, insulation stands 40~60min;
D. the obtained mixed liquors of step c are cooled to 35~45 DEG C, add absolute ethyl alcohol, centrifuge to obtain sediment, then with nothing Water-ethanol washs, and centrifuges, and dries, and obtains the nano zine oxide that particle diameter is 8~10nm.
Further, the weight of zinc nitrate and sodium carbonate ratio is (1.2~1.6) in the step a:1.
Further, white depositions and the solid-to-liquid ratio of lauryl glucosyl are 1g in the step b:(10~12) ml。
Further, white depositions and the solid-to-liquid ratio of trimethylol-propane trimethacrylate are in the step b 1g:(6~8) ml.
Further, the preparation method of the amido sodium lignin sulfonate is:
A. it is 65~75% sodium lignin sulfonate water by the sodium lignin sulfonate mass percent concentration soluble in water that is configured to Solution, 60~80 DEG C are heated to, add triethylene tetramine, it is water-soluble that the glutaraldehyde that mass percent concentration is 50% is then added dropwise Liquid, the drop rate of the glutaraldehyde water solution are 0.3~0.5mL/min, and time for adding control is in 20~30min, in temperature For 80~90 DEG C of 2~3h of reaction, amido lignin sulfonic acid sodium solution is obtained;
B. the amido lignin sulfonic acid sodium solution that step A is obtained is stripped with absolute ethyl alcohol, obtains extract, use oil Ether washs extract, is freeze-dried, produced after washing.
Further, the addition of the triethylene tetramine in the step A is lignin sulfonic acid sodium water solution cumulative volume 20~30%.
Further, the condition being freeze-dried in the step B is:- 8 DEG C of 2~4h of pre-freeze, it is then 0.04 in vacuum ~0.06mPa, temperature are -18 DEG C of 20~24h of freezing.
In addition, present invention also offers a kind of preparation method of the filter membrane for filtrating leukocytes, comprise the following steps:
Sodium alginate is added to the water by S1, stirs to being completely dissolved, obtains sodium alginate aqueous solution;
Chitosan oligosaccharide and amido sodium lignin sulfonate are added to the water by S2, stir to being completely dissolved, obtain mixed liquor;
Nano zine oxide is added to the water by S3, stirs to being completely dissolved, obtains nano oxidized zinc solution;
S4 mixes the mixed liquor that step S2 is obtained with the obtained sodium alginate aqueous solutions of step S1, stirs, must spin Silk solution, the spinneret orifice for being then 0.08mm by aperture with measuring pump are squeezed into the nano oxidized zinc solution that step S3 is obtained, Drawing-off, with 95% Ethanol Treatment fiber, centrifugation is sloughed drying fibrous after ethanol, is cut, is combed, networking, it is 4~3 μ that aperture, which is made, M network structure, is produced.
Filter membrane provided by the present invention for filtrating leukocytes is the aqueous solution by chitosan oligosaccharide and amido sodium lignin sulfonate Uniform spinning solution is formed after being blended with sodium alginate aqueous solution, is squeezed into burnett's solution and is prepared by spinneret orifice, Solve in the prior art by the way that the effect that polymeric material is grafted or is bonded is coated on hydrophobic carrier, it is white thin in filtering The polymer occurred during born of the same parents, which comes off, influences filter effect, or Leaching rule contaminated blood defect, and original provided by the invention Material is nontoxic, free of contamination composition, is a kind of environmentally friendly, healthy, free of contamination leukocyte filter membranes.
Double filtration principle is used provided by the present invention for the filter membrane of filtrating leukocytes, can effectively improve leucocyte With hematoblastic rejection rate.Aperture provided by the invention is the leukocyte filter membranes of 3~4 μm of network structure, can be prevented white thin Born of the same parents by the way that while the positive charge amido of positively charged chitosan oligosaccharide and the amido sodium lignin sulfonate on filter membrane has to leucocyte Very strong suction-operated, the two is acted on simultaneously, can effectively improve the rejection rate of leucocyte.In addition, embedded with self-control nano oxygen The sodium alginate fiber for changing zinc can have suction-operated with activated blood platelet to blood platelet, also have, in amido sodium lignin sulfonate The negatively charged groups such as the phenolic hydroxyl group that contains, alcoholic extract hydroxyl group, carbonyl, carboxyl can also activated blood platelet, also have to blood platelet and inhale Attached effect, the two is acted on simultaneously, can effectively improve hematoblastic filter out.
Further, through experiment find, provided by the present invention for filtrating leukocytes filter membrane to the leucocyte in whole blood Rejection rate be up to 99.999%, to hematoblastic rejection rate in whole blood up to more than 94%, it is white that its filtration result exceeded for the 3rd generation The requirement of cell filter, it is a kind of efficient leucocyte and hematoblastic cell filtration film.
Provided by the present invention for the self-control nano zine oxide in the filter membrane of filtrating leukocytes, chitosan oligosaccharide and amination amido wood The interaction of quality sodium sulfonate, which has, prevents filter membrane long-time from filtering generation filter opening and blocking, and alleviates and anti-Hemostatic Oral Liquid condenses the hair collected Raw effect, solving the modern aperture that the leukocyte depletion filter that network structure forms is formed by synthetic microfibril can detention morphotropism Poor cell, the red blood cell of modified difference and destroyed red blood cell are accumulated easily in leucocyte filter disc so that red in transfering bag Cell can not be by filter disc, while due also to blood sample inventory time is longer, causes the deformation of the viscosity and red blood cell of blood Property improve, the phenomenon of condensation collection occurs for blood, causes blood through occurring Severe blockage during leucocyte filter disc, causes filtering not smooth very To not dripping, the defects of hemofiltration time lengthening or endless blood filtration, the filter quality of blood leucocyte can be effectively guaranteed.
Further, find through experiment, 400mL whole bloods were carried out provided by the present invention for the filter membrane of filtrating leukocytes 14~16min is only needed during filter, illustrating the leukocyte filter membranes of the offer of the present invention has preferable hydrophilic wettability, is advantageous to blood The filtering of liquid.Meanwhile be 15~17min for the filtration time of the blood sample of exception, the time base with filtering normal blood This holding is constant, illustrates self-control nano zine oxide, chitosan oligosaccharide and amine in the filter membrane provided by the present invention for filtrating leukocytes Changing the interaction of amido sodium lignin sulfonate can prevent the aperture of filter membrane from blocking, and alleviate blood clotting phenomenon, can be effective Expand the use range of leukocyte filter membranes and increase the service life.
In addition, the sodium alginate cellulose provided by the invention containing self-control nano zine oxide and chitosan oligosaccharide interaction tool There is stronger antibacterial, sterilization, by germ contamination when can prevent blood filtration, while the fresh of blood can also be kept Degree, the security of filtering blood can be improved.
Compared with prior art, had the advantage that provided by the present invention for the filter membrane of filtrating leukocytes:
(1) filter membrane provided by the present invention for filtrating leukocytes has the advantages of adhesion is strong and stability is high, makes The material on filter membrane can be avoided to wash out or come off during, can effectively anti-Hemostatic Oral Liquid pollution;
(2) filter membrane provided by the present invention for filtrating leukocytes has leucocyte and blood platelet filtration rate high, in blood There is alleviation or anti-Hemostatic Oral Liquid cold agglutination phenomenon, the effect that dredging filter sizes block occurs during filtering, it is ensured that The filter quality of blood leucocyte, the service life length of leukocyte filter membranes can also be extended, be a kind of ideal leucocyte Filter membrane.
Embodiment:
Below by way of the description of embodiment, the invention will be further described, but this is not the limit to the present invention System, those skilled in the art according to the present invention basic thought, various modifications may be made or improve, but without departing from this The basic thought of invention, within the scope of the present invention.
Embodiment 1, a kind of preparation of nano zine oxide
A. weigh zinc nitrate to add in deionized water, stir to being completely dissolved, be subsequently added into sodium carbonate, the zinc nitrate with The weight ratio of sodium carbonate is 1.4:1, stirring centrifugation, obtains white depositions to reacting complete;
B. lauryl glucosyl is added toward the obtained white depositions of step a, stirs 6min, the white depositions Solid-to-liquid ratio with lauryl glucosyl is 1g:12ml, trimethylol-propane trimethacrylate is subsequently added into, stirred The solid-to-liquid ratio of 15min, the white depositions and trimethylol-propane trimethacrylate is 1g:8ml, obtain mixed liquor;
C. the obtained mixed liquors of step b are heated to 135 DEG C, insulation stands 35min, is then passed through nitrogen, continues to heat To 280 DEG C, insulation stands 50min;
D. the obtained mixed liquors of step c are cooled to 40 DEG C, add absolute ethyl alcohol, centrifuge to obtain sediment, then with anhydrous second Alcohol washs, and centrifuges, and dries, and obtains the nano zine oxide that particle diameter is 8~10nm.
Embodiment 2, a kind of preparation of amido sodium lignin sulfonate
A. it is 70% lignin sulfonic acid sodium water solution by the sodium lignin sulfonate mass percent concentration soluble in water that is configured to, 70 DEG C are heated to, adds triethylene tetramine, the addition of the triethylene tetramine is lignin sulfonic acid sodium water solution cumulative volume 25%, the glutaraldehyde water solution that mass percent concentration is 50% is then added dropwise, the drop rate of the glutaraldehyde water solution is 0.4mL/min, time for adding are controlled in 25min, are 85 DEG C of reaction 2h in temperature, are obtained amido lignin sulfonic acid sodium solution;
B. the amido lignin sulfonic acid sodium solution that step A is obtained is stripped with absolute ethyl alcohol, obtains extract, use oil Ether washs extract, is then 0.05mPa in vacuum, temperature is -18 DEG C of freezing 22h, i.e., in -8 DEG C of pre-freeze 3h after washing .
Embodiment 3, a kind of filter membrane for filtrating leukocytes
The filter membrane for filtrating leukocytes is made up of following preparing raw material and its parts by weight:
10 parts of 100 parts of sodium alginate, 35 parts of nano zine oxide, 15 parts of chitosan oligosaccharide and amido sodium lignin sulfonate;It is described to receive Rice zinc oxide is nano zine oxide prepared by embodiment 1, and the amido sodium lignin sulfonate is that amido prepared by embodiment 2 is wooden Plain sodium sulfonate.
Preparation method:
Sodium alginate is added to the water by S1, stirs to being completely dissolved, obtains sodium alginate aqueous solution;
Chitosan oligosaccharide and amido sodium lignin sulfonate are added to the water by S2, stir to being completely dissolved, obtain mixed liquor;
Nano zine oxide is added to the water by S3, stirs to being completely dissolved, obtains nano oxidized zinc solution;
S4 mixes the mixed liquor that step S2 is obtained with the obtained sodium alginate aqueous solutions of step S1, stirs, must spin Silk solution, the spinneret orifice for being then 0.08mm by aperture with measuring pump are squeezed into the nano oxidized zinc solution that step S3 is obtained, Drawing-off, with 95% Ethanol Treatment fiber, drying fibrous, cutting after ethanol is sloughed in centrifugation, and combing, networking, it is 3 μm that aperture, which is made, Network structure, produce.
Embodiment 4, a kind of filter membrane for filtrating leukocytes
The filter membrane for filtrating leukocytes is made up of following preparing raw material and its parts by weight:
15 parts of 160 parts of sodium alginate, 38 parts of nano zine oxide, 22 parts of chitosan oligosaccharide and amido sodium lignin sulfonate;It is described to receive Rice zinc oxide is nano zine oxide prepared by embodiment 1, and the amido sodium lignin sulfonate is that amido prepared by embodiment 2 is wooden Plain sodium sulfonate.
Preparation method is similar to Example 3.
Embodiment 5, a kind of filter membrane for filtrating leukocytes
The filter membrane for filtrating leukocytes is made up of following preparing raw material and its parts by weight:
20 parts of 200 parts of sodium alginate, 45 parts of nano zine oxide, 25 parts of chitosan oligosaccharide and amido sodium lignin sulfonate;It is described to receive Rice zinc oxide is nano zine oxide prepared by embodiment 1, and the amido sodium lignin sulfonate is that amido prepared by embodiment 2 is wooden Plain sodium sulfonate.
Preparation method is similar to Example 3.
Comparative example 1, a kind of filter membrane for filtrating leukocytes
The filter membrane for filtrating leukocytes is made up of following preparing raw material and its parts by weight:
15 parts of 160 parts of sodium alginate, 38 parts of nano zine oxide, 22 parts of chitosan oligosaccharide and amido sodium lignin sulfonate;It is described to receive Rice zinc oxide is commercially available nano zine oxide (being purchased from Beijing Deco Dao Jin Science and Technology Ltd.s, ZnO 30nm 99.9%), the amine Base sodium lignin sulfonate is amido sodium lignin sulfonate prepared by embodiment 2.
Preparation method is similar to Example 3.
Comparative example 2, a kind of filter membrane for filtrating leukocytes
The filter membrane for filtrating leukocytes is made up of following preparing raw material and its parts by weight:
15 parts of 160 parts of sodium alginate, 38 parts of nano zine oxide, 22 parts of chitosan and amido sodium lignin sulfonate;It is described to receive Rice zinc oxide is nano zine oxide prepared by embodiment 1, and the amido sodium lignin sulfonate is that amido prepared by embodiment 2 is wooden Plain sodium sulfonate.
Preparation method is similar to Example 3.
Difference with embodiment 4 is:Chitosan oligosaccharide is replaced with into chitosan.
Comparative example 3, a kind of filter membrane for filtrating leukocytes
The filter membrane for filtrating leukocytes is made up of following preparing raw material and its parts by weight:
160 parts of sodium alginate, 38 parts of nano zine oxide, 22 parts of chitosan oligosaccharide and acrylic acid-acrylic acid hydroxypropyl acrylate copolymer 15 Part;The nano zine oxide is nano zine oxide prepared by embodiment 1.
Preparation method is similar to Example 3.
Difference with embodiment 4 is:Amido sodium lignin sulfonate is replaced with into the copolymerization of acrylic acid-acrylic acid hydroxypropyl acrylate Thing.
Comparative example 4, a kind of filter membrane for filtrating leukocytes
The filter membrane for filtrating leukocytes is made up of following preparing raw material and its parts by weight:
15 parts of 160 parts of sodium alginate, 38 parts of nano zine oxide, 22 parts of chitosan oligosaccharide and sodium lignin sulfonate;The nano oxygen It is nano zine oxide prepared by embodiment 1 to change zinc.
Preparation method is similar to Example 3.
Difference with embodiment 4 is:Amido sodium lignin sulfonate is replaced with into sodium lignin sulfonate.
Test example one, the cell for the filter membrane of filtrating leukocytes filter effect test
1st, test material:Embodiment 3, embodiment 4, embodiment 5, comparative example 1, comparative example 2, comparative example 3 and comparative example 4 are made The standby filter membrane for filtrating leukocytes.
2nd, test method:
It is used for prepared by embodiment 3, embodiment 4, embodiment 5, comparative example 1, comparative example 2, comparative example 3 and comparative example 4 The filter membrane of filtrating leukocytes carries out on-line filtration to 400ml whole bloods, and evaluation leukocyte filter membranes remove leucocyte-removing and hematoblastic effect Fruit, leucocyte and platelet counts in forward and backward whole blood are filtered using blood-counter system measure, measures mistake in 400ml whole bloods The quantity for filtering proleukocyte is 2.5 × 109, the quantity for filtering thromboblast is 8 × 1010
The assay method of wherein remaining leukocyte count is:By in the test tube of the whole blood sampling after filtering to polyethylene, with After acridine orange liquid dyes the leucocyte spilt, it is measured with fluorescence microscope.The white blood cell concentration of measure is multiplied by recovery Whole blood liquid measure, measure in collection bag contained remaining leukocyte count.
Leucocyte (blood platelet) rejection rate (%)=L0-L1/L0× 100, wherein L0To contain before filtering in unit volume whole blood Some leucocyte (blood platelet) quantity, L1For leucocyte (blood platelet) quantity contained in unit volume whole blood after filtering.
3rd, result of the test:
Result of the test is as shown in table 1.
Table 1 is used for the filter membrane of filtrating leukocytes to leucocyte and hematoblastic filtration result
As shown in Table 1, the filter membrane for filtrating leukocytes that prepared by the embodiment of the present invention 3~5 is to the leucocyte in whole blood It is respectively provided with blood platelet and preferably filters out efficiency, wherein being up to 99.999% to the rejection rate of leucocyte, is filtered out to hematoblastic Rate is significantly better than the filter membrane for filtrating leukocytes of example 1-4 preparations by contrast to the leucocyte in whole blood up to more than 94% With hematoblastic rejection rate, its filtration result has exceeded the requirement of the 3rd generation leucocyte filter.
Test example two, the filter opening plugging performance for the filter membrane of filtrating leukocytes detect experiment
1st, test material:Embodiment 3, embodiment 4, embodiment 5, comparative example 1, comparative example 2, comparative example 3 and comparative example 4 are made The standby filter membrane for filtrating leukocytes.
2nd, test method:
The use prepared using embodiment 3, embodiment 4, embodiment 5, comparative example 1, comparative example 2, comparative example 3 and comparative example 4 In filtrating leukocytes filter membrane in the blood warehousing of storehouse the time it is longer, the high shear viscosity of blood is 4.8mPa.s after testing, in cut Viscosity is 5.3mPa.s, low shear viscosity 10.5mPa.s, HCT 0.43%, and the abnormal blood that AI 2.34, IR are 0.53 is Sample is detected, blood sample sampling 400ml, records each blood mistake with 400ml normal healths blood sample as a control group Filter the time.
3rd, result of the test:
Result of the test is as shown in table 2.
Filtration time of the filter membrane of table 2 to whole blood
As shown in Table 2, the filter membrane for filtrating leukocytes being prepared using the embodiment of the present invention 3~4 is complete to 400mL Blood, which filter, only needs 14~16min, illustrates the filter membrane for filtrating leukocytes of the offer of the present invention and has preferably parent Water wettability, be advantageous to the filtering of blood.Meanwhile be 15~17min for the filtration time of the blood sample of exception, with filtering The time of normal blood is held essentially constant, and the membrane filtration for filtrating leukocytes that comparative example 1~4 is prepared is abnormal Blood sample at least extends the time of more than half, or even the phenomenon that can not be filtered occurs, illustrate provided by the present invention for Self-control nano zine oxide, chitosan oligosaccharide in the filter membrane of filtrating leukocytes and the interaction of amination amido sodium lignin sulfonate can be to prevent Only the aperture of filter membrane blocks, and alleviates blood clotting phenomenon, can effectively expand the use range of leukocyte filter membranes.

Claims (9)

1. a kind of filter membrane for filtrating leukocytes, it is characterised in that including following preparing raw material and its parts by weight:Alginic acid 10~20 parts of 100~200 parts of sodium, 35~45 parts of nano zine oxide, 15~25 parts of chitosan oligosaccharide and amido sodium lignin sulfonate;
The preparation method of the amido sodium lignin sulfonate is:
A. it is 65~75% lignin sulfonic acid sodium water solutions by the sodium lignin sulfonate mass percent concentration soluble in water that is configured to, 60~80 DEG C are heated to, adds triethylene tetramine, the glutaraldehyde water solution that mass percent concentration is 50% is then added dropwise, it is described The drop rate of glutaraldehyde water solution is 0.3~0.5mL/min, and time for adding is controlled in 20~30min, is 80~90 in temperature DEG C reaction 2~3h, obtain amido lignin sulfonic acid sodium solution;
B. the amido lignin sulfonic acid sodium solution that step A is obtained is stripped with absolute ethyl alcohol, obtains extract, washed with petroleum ether Extract is washed, is freeze-dried, produced after washing.
2. it is used for the filter membrane of filtrating leukocytes as claimed in claim 1, it is characterised in that including following preparing raw material and its again Measure number:
15 parts of 160 parts of sodium alginate, 38 parts of nano zine oxide, 22 parts of chitosan oligosaccharide and amido sodium lignin sulfonate.
3. it is used for the filter membrane of filtrating leukocytes as claimed in claim 1, it is characterised in that the preparation side of the nano zine oxide Method is:
A. weighing zinc nitrate to add in deionized water, stir to being completely dissolved, be subsequently added into sodium carbonate, stirring is complete to reaction, Centrifugation, obtains white depositions;
B. lauryl glucosyl is added in the white depositions obtained toward step a, 5~8min is stirred, is subsequently added into three hydroxyls Trimethacrylate, 10~20min is stirred, obtains mixed liquor;
C. the obtained mixed liquors of step b are heated to 130~140 DEG C, insulation stands 30~40min, is then passed through nitrogen, continues 250~300 DEG C are heated to, insulation stands 40~60min;
D. the obtained mixed liquors of step c are cooled to 35~45 DEG C, add absolute ethyl alcohol, centrifuge to obtain sediment, then with anhydrous second Alcohol washs, and centrifuges, and dries, and obtains the nano zine oxide that particle diameter is 8~10nm.
4. it is used for the filter membrane of filtrating leukocytes as claimed in claim 3, it is characterised in that zinc nitrate and carbon in the step a The weight ratio of sour sodium is (1.2~1.6):1.
5. it is used for the filter membrane of filtrating leukocytes as claimed in claim 3, it is characterised in that white depositions in the step b Solid-to-liquid ratio with lauryl glucosyl is 1g:(10~12) ml.
6. it is used for the filter membrane of filtrating leukocytes as claimed in claim 3, it is characterised in that white depositions in the step b Solid-to-liquid ratio with trimethylol-propane trimethacrylate is 1g:(6~8) ml.
7. it is used for the filter membrane of filtrating leukocytes as claimed in claim 1, it is characterised in that the triethylene four in the step A The addition of amine is the 20~30% of lignin sulfonic acid sodium water solution cumulative volume.
8. it is used for the filter membrane of filtrating leukocytes as claimed in claim 1, it is characterised in that be freeze-dried in the step B Condition is:- 8 DEG C of 2~4h of pre-freeze, it is then 0.04~0.06mPa in vacuum, temperature is -18 DEG C of 20~24h of freezing.
9. the preparation method of the filter membrane for filtrating leukocytes as described in claim 1-8 is any, it is characterised in that including with Lower step:
Sodium alginate is added to the water by S1, stirs to being completely dissolved, obtains sodium alginate aqueous solution;
Chitosan oligosaccharide and amido sodium lignin sulfonate are added to the water by S2, stir to being completely dissolved, obtain mixed liquor;
Nano zine oxide is added to the water by S3, stirs to being completely dissolved, obtains nano oxidized zinc solution;
S4 mixes the mixed liquor that step S2 is obtained with the obtained sodium alginate aqueous solutions of step S1, stirs, it is molten to obtain spinning Liquid, the spinneret orifice for being then 0.08mm by aperture with measuring pump are squeezed into the nano oxidized zinc solution that step S3 is obtained, drawing-off, With 95% Ethanol Treatment fiber, centrifugation sloughs drying fibrous, cutting after ethanol, combing, networking, the net that aperture is 4~3 μm is made Shape structure, is produced.
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