CN107649102A - A kind of preparation method of compound doughnut polymeric adsorbent - Google Patents
A kind of preparation method of compound doughnut polymeric adsorbent Download PDFInfo
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- CN107649102A CN107649102A CN201710916906.1A CN201710916906A CN107649102A CN 107649102 A CN107649102 A CN 107649102A CN 201710916906 A CN201710916906 A CN 201710916906A CN 107649102 A CN107649102 A CN 107649102A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES 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
- A61M1/00—Suction or pumping devices for medical purposes; Devices for carrying-off, for treatment of, or for carrying-over, body-liquids; Drainage systems
- A61M1/02—Blood transfusion apparatus
- A61M1/0272—Apparatus for treatment of blood or blood constituents prior to or for conservation, e.g. freezing, drying or centrifuging
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
- B01J20/28038—Membranes or mats made from fibers or filaments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28095—Shape or type of pores, voids, channels, ducts
- B01J20/28097—Shape or type of pores, voids, channels, ducts being coated, filled or plugged with specific compounds
Abstract
The present invention relates to a kind of, preparation method of compound doughnut polymeric adsorbent, and it comprises the following steps：Take the ethanol solution processing that macroreticular resin is put, macroreticular resin emulsion after processing is thrown into the above-mentioned ps hollow fiber uf membrane being soaked in deionized water, sonic oscillation processing, until above-mentioned emulsion is fully injected into inside ps hollow fiber uf membrane, sealing treatment is carried out after ps hollow fiber uf membrane is dried, is then soaked in physiological saline, doughnut cladding adsorptive resin is obtained after dry sterilization, hydrophilic modifying processing is finally carried out, required compound doughnut polymeric adsorbent is obtained after dry sterilization.Compared with prior art, the filling rate of macroreticular resin is up to 100%~200% in the compound doughnut polymeric adsorbent that in the present invention prepared by preparation method of the invention, it can remove the unwanted metabolic products such as lactic acid caused by blood product in real time, Erythrocyte preservation damage can effectively be alleviated, improve red cell preservation quality.
Description
Technical field
The present invention relates to blood purification and chemical field, more particularly to a kind of compound doughnut polymeric adsorbent
Preparation method.
Background technology
Red blood cell can gradually produce Physiology and biochemistry change in storage process, and accumulate some potential detrimental metabolic productions
Thing, this process are referred to as " Erythrocyte preservation damage ".Erythrocyte preservation damage is mainly shown as that PH is reduced, ATP in red blood cell
And 2,3-DPG are reduced, red blood cell vesica is formed, protein and lipid oxidation, S-nitrosoglutathione decreased hemoglobin, cell surface saliva
Liquid acid is lost, and CD47 expression is reduced, and phosphatidylserine (PS) turns up and erythrocyte deformability reduces, and is ultimately resulted in red thin
Born of the same parents' oxygen carrying capacity declines, and is easy to by macrophage removing and the generation of Adverse transfusion reaction.
The life-span average out to of red blood cell 120 days, but can only store in vitro 35 days or so, and after storing two weeks i.e.
Obvious red cell morphology function can be observed to change, thus caused Adverse transfusion reaction also substantially increases.With it is red thin in vivo
Born of the same parents' metabolite timely and effective can remove difference, and the particularly lactic acid accumulation of unwanted metabolic products caused by storage of red blood cells is recognized
To be the early stage inducement of Erythrocyte preservation damage, Enzyme activity in red blood cell causes energy metabolism impairment, ATP extremely under sour environment
Content reduces to be destroyed so as to trigger a series of chain effect to ultimately result in erythrocytolysis, and largely harmful generation caused by haemolysis
Thank to the damage that product has further aggravated red blood cell.
The unwanted metabolic products such as caused inflammatory factor, free hemoglobin, iron ion have during Erythrocyte preservation
There is potential immunoregulation effect, and these immunoregulation effects are mainly shown as that blood transfusion related immune suppresses, and may cause to feel
Incidence increase is contaminated, metastases and recurrence rate increase, and MOFE, or even receptor are dead.Proteomics is ground
Discovery is studied carefully with the increase of period of storage, and the unwanted metabolic products in preserved blood substantially increase, leucocyte release, Erythrocyte Damage
And plasma protein composition degraded is its main source.The generation of adverse reaction is with being transfused after clinical research discovery red blood cell transfusion
The period of storage of red blood cell is relevant, and its mechanism is probably because the unwanted metabolic products of accumulation are largely discharged in infusion process
To recipient's body, because the foundation of proinflammatory tissue microenvironment causes the change of immune regulation mechanism so as to trigger Adverse transfusion reaction
Generation.
Research finds, sFas Ligand (sFasL), Soluble ICAM-1 (sICAM- in preserved blood
1), soluble human leukocyte antigens-I (sHLA- I), soluble CD 40 ligand (sCD40L), IL-6, IL-8, TGF-β 1,
The bioactive substances such as RNATES suppress closely related with blood transfusion related immune, and it is mainly by leucocyte in storage process and blood
Produced by platelet discharges or degraded；Kassinin kinin, complement, histamine, immunoglobulin fragments are mainly derived from the activation of plasma protein, drop
Solution；Hematoclasis can produce substantial amounts of superoxide dismutase and bilirubin material；Above-mentioned substance may aggravate red blood cell
Storage lesion.
In summary, due to the acidic materials such as lactic acid, pyruvic acid accumulation during Erythrocyte preservation, medium for storing PH is caused
Decline, influence the energetic supersession of red blood cell, cause the oxidative damage of red blood cell, dissolved destruction.And caused by Erythrocyte Damage
Free hemoglobin, iron ion, serum potassium, inflammatory factor and Erythrocytes Aged in vitro enter in receptor's body so as to cause blood transfusion not
The generation of good reaction.
At present, studies have found that：Adsorptive resin is coated using hollow polysulfone fibre, effectively can both adsorb in blood has
Malicious harmful substance, there is blood complimentary nature again, the adverse consequences such as haemolysis, PH changes will not occur, can effectively solve existing
The problem of blood storage means are present, such as：(application publication number is CN 106238023 to Application No. 201610705333.3
A a kind of coating method for being used to improve blood purification material surface biocompatibility) is disclosed.However, using existing method
The hollow polysulfone fibre cladding adsorptive resin prepared, filling rate of the adsorptive resin in hollow polysulfone fibre is relatively low, so as to
Influence to the treatment effect of blood sample, on the other hand, the compatibility of itself and blood need to be improved.
The content of the invention
First technical problem to be solved by this invention is to provide a kind of polymeric adsorbent filling rate for prior art
The preparation method of high compound doughnut polymeric adsorbent.
It is good that second technical problem to be solved by this invention provides a kind of blood compatibility for prior art
The preparation method of compound doughnut polymeric adsorbent.
Technical scheme is used by the present invention solves above-mentioned technical problem：A kind of compound doughnut polymeric adsorbent
Preparation method, it is characterised in that comprise the following steps：
(1) take macroreticular resin to be placed in the ethanol solution that concentration is 30~45%, stirring 2~3h of immersion, macropore tree is made
The mass volume ratio of fat emulsion, wherein macroreticular resin and ethanol solution is 4~5:100~150g/ml；
(2) a certain amount of ps hollow fiber uf membrane is taken to be soaked in 10~15min in deionized water；
(3) the macroreticular resin emulsion of above-mentioned preparation is thrown to the above-mentioned ps hollow fiber uf membrane being soaked in deionized water
In, sonic oscillation processing, until above-mentioned emulsion is fully injected into inside ps hollow fiber uf membrane, wherein in macroreticular resin and polysulfones
The mass ratio of empty fiber membrane is 1~2:1, wherein, when the ethanol solution of macroreticular resin mixes with ps hollow fiber uf membrane, ethanol point
Son can in water diffusion mobility and drive macroreticular resin enter ps hollow fiber uf membrane inside, so as to improve ps hollow fiber uf membrane
The filling rate of middle macroreticular resin.
(4) sealing part will be carried out to it using polysulfones solution after the ps hollow fiber uf membrane of step (3) processing is dried
Reason；
(5) ps hollow fiber uf membrane after above-mentioned sealing is soaked in physiological saline after 6~7d, dry sterilization, in obtaining
Hollow fiber coats adsorptive resin；
(6) the doughnut cladding adsorptive resin of above-mentioned preparation is subjected to hydrophilic modifying processing, institute is obtained after dry sterilization
The compound doughnut polymeric adsorbent needed.
Preferably, the hydrophilic modifying processing comprises the following steps：
(1) a certain amount of hydrophilic modifier, surface fixative and initiator are dissolved in triethyl phosphate, are completely dissolved
Afterwards, under nitrogen protection, 80~85 DEG C of 18~20h of reaction, prepolymer P is obtained, wherein above-mentioned hydrophilic modifier, surface fixative, drawing
The mass ratio for sending out agent and triethyl phosphate is 7~8:5~6:0.1~0.2:180~220；
(2) by above-mentioned prepolymer P and deionized water with volume ratio 1~1.5:1 is well mixed to obtain modified solution；
(3) above-mentioned doughnut cladding adsorptive resin is immersed in above-mentioned modified solution, stirring immersion 1.5~
2.0h, until doughnut cladding adsorptive resin microswelling；
(4) the doughnut cladding adsorptive resin of microswelling is taken out from modified solution, being dipped to concentration again is
In 1.0~1.5wt.% citric acid solution, 8~10h of hydrolysis process at 55~60 DEG C；Wherein citric acid solution can promote above-mentioned
Prepolymer P coats the cross-linked polymeric on adsorptive resin surface in doughnut, so as to promote hydrophilic modifying effect.
(5) film through lemon acid soak is put into physiological saline, soaks 3~4d, after dry sterilization it is required compound
Type doughnut polymeric adsorbent.Finally compound doughnut polymeric adsorbent and blood can be provided using physiological saline immersion treatment
Identical osmotic pressure environment, so as to improve the biocompatibility of compound doughnut polymeric adsorbent and blood, be advantageous to the material
Material and contacting blood.
Preferably, the preparation method of the polysulfones particle in the step (4) is：By polysulfones grain dissolution and organic solvent
In, 20~25h is stirred under the conditions of 75~80 DEG C, polysulfones solution is obtained, wherein the mass ratio of above-mentioned polysulfones particle and organic solvent
For 1:4~5, above-mentioned organic solvent is one kind in 1-METHYLPYRROLIDONE, dimethyl acetamide or DMF.
Preferably, the macroreticular resin is porous poly- to benzene divinyl microballoon, it is porous poly- to benzene divinyl microsphere surface
With basic group, intermolecular weak interaction can be produced with the metabolic waste in blood, be fixed in resin surface, this
Outside, this it is porous it is poly- there is loose structure to benzene divinyl microballoon, there is larger surface area, and then there is larger adsorbance.
Preferably, the macroreticular resin is at least one of XT30 or fpa 90ci.
Preferably, the condition of the sonic oscillation processing is：Ultrasonic frequency is 40~50KHz, and temperature is 25~30
℃。
Preferably, the hydrophilic modifier contains pyrrolidone group and carbon-carbon double bond group, wherein pyrrolidones energy
Hydrophily is provided, and carbon-carbon double bond is radical reaction functional group.
Further, it is preferable that the hydrophilic modifier is vinyl pyrrolidone.
Preferably, the surface fixative contains carbon-carbon double bond group and ethoxysilane groups, or contain carbon carbon
Double bond group and methoxy silane groups.
Further, it is preferable that the surface fixative is VTES or vinyltrimethoxy silane
At least one of.
Compared with prior art, the advantage of the invention is that：Certain density ethanol is used in the preparation method of the present invention
Solution is handled macroreticular resin, is then mixed it with ps hollow fiber uf membrane, can not only increase polysulfone hollow fibre
The aperture on film surface, and in both mixed processes, ethanol molecule diffusive migration and can drive macroreticular resin to carry out in water
Inside ps hollow fiber uf membrane, so as to improve the filling rate of macroreticular resin in ps hollow fiber uf membrane, in addition, ultrasonication energy
Further promote macroreticular resin to ps hollow fiber uf membrane internal migration, so as to which further macroreticular resin is in ps hollow fiber uf membrane
In filling rate.
By the filling rate of macroreticular resin in the compound doughnut polymeric adsorbent for preparing of the present invention up to 100%~
200%, it can remove the unwanted metabolic products such as lactic acid caused by blood product in real time, can effectively alleviate Erythrocyte preservation damage
Wound, improve red cell preservation quality.
Brief description of the drawings
Fig. 1 is the blood compatibility result of study of hollow fiber polysulfone membrane and different materials in the embodiment of the present invention；
Fig. 2 is the leukocyte activation release experiment result of compound doughnut polymeric adsorbent in the embodiment of the present invention, its
Middle XF is compound doughnut polymeric adsorbent, similarly hereinafter；
Fig. 3 is influence of the compound doughnut polymeric adsorbent to blood storage quality in the embodiment of the present invention, wherein, A,
B, C, D, E are respectively the change of pH value, lactic acid, free hemoglobin, ATP, 2,3-DPG content and blood potassium；
Fig. 4 is influence of the compound doughnut polymeric adsorbent to blood mesobilirubin content in the embodiment of the present invention；
Fig. 5 is compound doughnut polymeric adsorbent in the embodiment of the present invention to immunoglobulin fragment content in blood
Influence；
Fig. 6 is influence of the compound doughnut polymeric adsorbent to complement content in blood in the embodiment of the present invention.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing embodiment.
Embodiment one：The preparation of compound doughnut polymeric adsorbent
Embodiment 1：
The ethanol solution that the concentration for taking XT30 (being purchased from the easy science and technology limited Company of the intelligent moral in Beijing, similarly hereinafter) to be placed in is 30%
In, stirring immersion 2h is made XT30 emulsion, and the mass volume ratio of wherein XT30 and ethanol solution is 4:100g/ml.Take certain
The ps hollow fiber uf membrane (Chinese Academy of Sciences's Ningbo material is provided, similarly hereinafter) of amount is soaked in 10min in deionized water, by above-mentioned preparation
XT30 emulsion throw into the above-mentioned ps hollow fiber uf membrane being soaked in deionized water, sonic oscillation processing, until above-mentioned
Emulsion is fully injected into inside ps hollow fiber uf membrane, and the mass ratio of wherein XT30 and ps hollow fiber uf membrane is 1:1, ultrasound is shaken
The condition for swinging processing is：Ultrasonic frequency is 40KHz, and temperature is 25 DEG C.
Ps hollow fiber uf membrane through above-mentioned processing is dried, carries out the sealing treatment (present invention to it using polysulfones solution
The middle sealing treatment method used is conventional method of the prior art).Wherein, the preparation method of polysulfones solution is：By polysulfones
Grain dissolution stirs 20h in 1-METHYLPYRROLIDONE under the conditions of 75 DEG C, obtain polysulfones solution, wherein above-mentioned polysulfones particle with
The mass ratio of organic solvent is 1:4.
Ps hollow fiber uf membrane after sealing treatment is soaked in 6d in physiological saline, doughnut bag is obtained after dry sterilization
Cover adsorptive resin.Hydrophilic modifying processing is carried out to the doughnut cladding adsorptive resin of above-mentioned preparation, obtained after dry sterilization
Required compound doughnut polymeric adsorbent.The process of wherein hydrophilic treated is：By vinyl pyrrolidone, the second of vinyl three
TMOS and azodiisobutyronitrile are dissolved in triethyl phosphate, after being completely dissolved, under nitrogen protection, 80 DEG C of reaction 18h, are obtained
Prepolymer P, wherein above-mentioned vinyl pyrrolidone, VTES, azodiisobutyronitrile and triethyl phosphate
Mass ratio be 7:5:0.1:180.Above-mentioned prepolymer P is well mixed with deionized water with volume ratio 1~1.5 must be modified it is molten
Liquid, above-mentioned doughnut cladding adsorptive resin is immersed in above-mentioned modified solution, stirring immersion 1.5h, until doughnut
Adsorptive resin microswelling is coated, then takes out the doughnut cladding adsorptive resin of microswelling from modified solution, then
It is secondary to be dipped in the citric acid solution that concentration is 1.0wt.%, hydrolysis process 8h at 55 DEG C, finally, by after lemon acid soak
Doughnut cladding adsorptive resin is put into physiological saline, soaks 3d, required compound doughnut is obtained after dry sterilization
Polymeric adsorbent.
Embodiment 2：
The concentration for taking XT30 to be placed in is in 40% ethanol solution, stirring immersion 2.5h, XT30 emulsion is made, wherein
The mass volume ratio of XT30 and ethanol solution is 4.5:125g/ml.A certain amount of ps hollow fiber uf membrane is taken to be soaked in deionization
12min in water, the XT30 emulsion of above-mentioned preparation is thrown into the above-mentioned ps hollow fiber uf membrane being soaked in deionized water, surpassed
Sound oscillation is handled, until above-mentioned emulsion is fully injected into inside ps hollow fiber uf membrane, wherein XT30 and ps hollow fiber uf membrane
Mass ratio be 1.5:1, sonic oscillation processing condition be：Ultrasonic frequency is 45KHz, and temperature is 27 DEG C.Will be through above-mentioned place
The ps hollow fiber uf membrane of reason is dried, and sealing treatment is carried out to it using polysulfones solution.Wherein, the preparation method of polysulfones solution
For：By polysulfones grain dissolution in dimethyl acetamide, 22h is stirred under the conditions of 77 DEG C, polysulfones solution is obtained, wherein above-mentioned polysulfones
The mass ratio of particle and organic solvent is 1:4.5.
Ps hollow fiber uf membrane after sealing treatment is soaked in 6.5d in physiological saline, doughnut is obtained after dry sterilization
Coat adsorptive resin.Hydrophilic modifying processing is carried out to the doughnut of above-mentioned preparation cladding adsorptive resin, after dry sterilization
Obtain required compound doughnut polymeric adsorbent.The process of wherein hydrophilic treated is：By vinyl pyrrolidone, vinyl three
Ethoxysilane and azodiisobutyronitrile are dissolved in triethyl phosphate, after being completely dissolved, under nitrogen protection, and 82 DEG C of reaction 19h,
Prepolymer P is obtained, wherein above-mentioned vinyl pyrrolidone, VTES, azodiisobutyronitrile and tricresyl phosphate second
The mass ratio of ester is 7.5:5.5:0.15:200.Above-mentioned prepolymer P is well mixed with deionized water with volume ratio 1~1.2
Modified solution, above-mentioned doughnut cladding adsorptive resin is immersed in above-mentioned modified solution, stirring immersion 1.7h, until in
Hollow fiber coats adsorptive resin microswelling, then takes the doughnut cladding adsorptive resin of microswelling from modified solution
Go out, be dipped to again in the citric acid solution that concentration is 1.2wt.%, hydrolysis process 9h at 57 DEG C finally, will be through lemon acidleach
Doughnut cladding adsorptive resin after bubble is put into physiological saline, soaks 3.5d, after dry sterilization it is required compound
Doughnut polymeric adsorbent.
Embodiment 3：
Fpa 90ci (being purchased from the intelligent benefit Science and Technology Ltd. in Beijing) are taken to be placed in the ethanol solution that concentration is 45%, stirring
3h is soaked, fpa 90ci emulsion is made, the wherein mass volume ratio of fpa 90ci and ethanol solution is 5:150g/ml.Take one
Quantitative ps hollow fiber uf membrane is soaked in 15min in deionized water, and the fpa 90ci emulsion of above-mentioned preparation is thrown to above-mentioned
It is soaked in the ps hollow fiber uf membrane in deionized water, sonic oscillation processing, until above-mentioned emulsion is fully injected into polysulfones
Inside empty fiber membrane, wherein the mass ratio of macroreticular resin and ps hollow fiber uf membrane is 2:1, sonic oscillation processing condition be：
Ultrasonic frequency is 50KHz, and temperature is 30 DEG C.
Ps hollow fiber uf membrane through above-mentioned processing is dried, sealing treatment is carried out to it using polysulfones solution.Wherein, gather
The preparation method of sulfolane solution is：By polysulfones grain dissolution in DMF, 25h is stirred under the conditions of 80 DEG C, is obtained
Polysulfones solution, wherein the mass ratio of above-mentioned polysulfones particle and organic solvent is 1:5.
Ps hollow fiber uf membrane after sealing treatment is soaked in 7d in physiological saline, doughnut bag is obtained after dry sterilization
Cover adsorptive resin.The doughnut cladding adsorptive resin of above-mentioned preparation carries out hydrophilic modifying processing, and institute is obtained after dry sterilization
The compound doughnut polymeric adsorbent needed.The process of wherein hydrophilic treated is：By vinyl pyrrolidone, the ethoxy of vinyl three
Base silane and azodiisobutyronitrile are dissolved in triethyl phosphate, after being completely dissolved, under nitrogen protection, 85 DEG C of reaction 120h, are obtained
Prepolymer P, wherein above-mentioned vinyl pyrrolidone, VTES, azodiisobutyronitrile and tricresyl phosphate
The mass ratio of ethyl ester is 8:6:0.2:220.By above-mentioned prepolymer P and deionized water with volume ratio 1.5:1 it is well mixed must be modified
Solution, above-mentioned doughnut cladding adsorptive resin is immersed in above-mentioned modified solution, stirring immersion 2.0h, until hollow fibre
Dimension cladding adsorptive resin microswelling, then the doughnut cladding adsorptive resin of microswelling is taken out from modified solution,
It is dipped to again in the citric acid solution that concentration is 1.5wt.%, hydrolysis process 10h at 60 DEG C finally, will be through lemon acid soak
Doughnut cladding adsorptive resin afterwards is put into physiological saline, soaks 4d, after dry sterilization it is required compound hollow
Fibers adsorption resin.
Embodiment two：Application study of the compound doughnut polymeric adsorbent of above-mentioned preparation in blood preseration
Reagent and instrument：
The blood gas analyzers of GEM Premier 4000 (the fertile sweet smell in the U.S.)；The resins of Amberchrom CG 300 (U.S. Luo Menha
This company)；Measurement of free-haemoglobin in plasma kit (Beijing riel reaches)；ELISpot kits (Beijing is biological up to section)；
2,3-DPG Elisa Kit (sing all biologies in Shanghai)；ATP assays kit (biology is built up in Nanjing)；AU5400 biochemical instruments
(U.S.'s Beckman)；IMMAGE800 analyzers (U.S.'s Beckman)；(TSCD- II, Japan are safe for the sterile catheter connection machines of TSCD- II
You are luxuriant).
Test specimen：
Blood sample (non-infectious reason scrap blood, being provided by Ningbo downtown blood station) is bisected into two parts, its
Middle a part of blood is added in the blood bag containing compound doughnut polymeric adsorbent of making number by sterile adapter, another
Part as a control group, preserves according to a conventional method.
Statistical procedures：
Data are handled using the statistics softwares of SPSS 13.0, are represented with mean ± standard deviation, are compared between group and examined using t,
P ＜ 0.05 have statistical significance.
Embodiment 1：Biocompatibility detects
By hollow fiber polysulfone membrane and other materials (including two kinds of non-woven fabrics, two kinds of nylon membranes and two kinds of acetate fibers
Film etc.) it is implanted to respectively in the blood product that anticoagulant for storage of whole blood is CPD, after 4 DEG C are stored 28 days, detect the blood red egg that dissociates in supernatant
White concentration, compares whether hollow fiber polysulfone membrane has more preferable biocompatibility compared with other materials, and control group is then normal
The blood product that rule method preserves.IL-1 β, IL-6, IFN-α are used to observe leukocyte activation release conditions, and blood can be used as saturating
Analyse the index of film biocompatibility quality.Blood product is mixed with compound doughnut polymeric adsorbent, blood bank's standard conditions
After lower 4 DEG C of storages 24 hours, separation leucocyte carries out ELISPOT experiment detection leucocyte releases IL-1 β, IL-6, IFN-α feelings
Condition, using undressed blood product as negative control, the blood product that non-woven fabrics b is implanted into is used as positive control.
Result of study shows hollow fiber polysulfone membrane group compared with Normal group, and there was no significant difference for haemolysis situation, with
Other each group materials are compared, and haemolysis situation is then obvious preferable, shows that Polysulfone hollow fibers have preferable biocompatibility, is protecting
Haemolysis (as shown in Figure 1) will not be caused by depositing in the phase.The compound doughnut polymeric adsorbent pair that ELISPOT experiment displays are made
Leucocyte has good biocompatibility, can used as preserved blood scavenging material (such as Fig. 2 institutes without obvious activation
Show).
Embodiment 2：Influence of the compound doughnut polymeric adsorbent to blood product quality
The index of correlation (PH, K+ and lactic acid etc.) of blood product is detected using blood gas analyzer；Swum using blood plasma
Free hemoglobin content is detected from hemoglobinometry kit, observes storage of red blood cells haemolysis situation.Detect difference simultaneously
Store red blood cell ATP and the 2,3-DPG changes of contents of period.Total bilirubin, immune globulin white tiles are detected using Biochemical Analyzer
Section (including IgG, IgA, IgM) and complement (including C3, C4) content.More than detection in strict accordance with instrument or kit illustrate into
Row operation.
Result of study shows that in compound whole blood of the doughnut polymeric adsorbent implantation containing CPD, storage finds storage after 28 days
Deposit blood and have no obvious haemolysis, its pH value has no obvious change, and lactic acid and other biological active material such as bilirubin, immune globulin
White tiles section, complement etc. significantly reduce compared with control group, ATP in red blood cell, 2,3-DPG contents apparently higher than control group (such as Fig. 3~
Shown in 6).So as to prove that the direct contact by deadening resin and red blood cell can avoid damaging action of the resin to haemocyte,
Contribute to improve Erythrocyte preservation quality simultaneously.By blood system of the compound doughnut polymeric adsorbent implantation containing different preservation liquid
In product, and extend the blood product shelf life, the results showed that the blood product for implanting compound doughnut polymeric adsorbent prolongs
After having grown certain period of storage, compared with control group, Erythrocyte preservation quality is preferable.
Embodiment 3：Compound doughnut polymeric adsorbent is to extending the Erythrocyte preservation time limit
The Erythrocyte preservation time limit depends on Quality of Erythrocyte, according to the studies above result, predicts and is store by removing red blood cell
Caused unwanted metabolic products can improve Erythrocyte preservation quality during depositing, so as to extend the Erythrocyte preservation time limit.For this
By the implantation of compound doughnut polymeric adsorbent containing different anticoagulant for storage of whole blood ACD (effective storage life be 21 days, be extended for 28 days),
CPD (effective storage life is 28 days, is extended for 35 days), CPPA-1 (effective storage life is 35 days, is extended for 42 days) blood product
In, continuously stored under standard blood bank conditions, collect blood sample weekly and carry out Quality of Erythrocyte detection, Testing index and method are same
On, whether the red blood cell of observation extension shelf life can still reach the quality requirement of red blood cell transfusion.
Claims (10)
1. a kind of preparation method of compound doughnut polymeric adsorbent, it is characterised in that comprise the following steps：
(1) take macroreticular resin to be placed in the ethanol solution that concentration is 30~45%, stirring 2~3h of immersion, macroreticular resin breast is made
The mass volume ratio of turbid, wherein macroreticular resin and ethanol solution is 4~5:100~150g/ml；
(2) a certain amount of ps hollow fiber uf membrane is taken to be soaked in 10~15min in deionized water；
(3) the macroreticular resin emulsion of above-mentioned preparation is thrown into the above-mentioned ps hollow fiber uf membrane being soaked in deionized water,
Sonic oscillation processing, until above-mentioned emulsion is fully injected into inside ps hollow fiber uf membrane, wherein macroreticular resin and polysulfone hollow
The mass ratio of tunica fibrosa is 1~2:1；
(4) sealing treatment will be carried out to it using polysulfones solution after the ps hollow fiber uf membrane of step (3) processing is dried；
(5) ps hollow fiber uf membrane after above-mentioned sealing is soaked in 6~7d in physiological saline, dry sterilization, obtains doughnut
Coat adsorptive resin；
(6) the doughnut cladding adsorptive resin of above-mentioned preparation is subjected to hydrophilic modifying processing, obtained after dry sterilization required
Compound doughnut polymeric adsorbent.
2. preparation method as claimed in claim 1, it is characterised in that the hydrophilic modifying processing comprises the following steps：
(1) hydrophilic modifier, surface fixative and initiator are dissolved in triethyl phosphate, after being completely dissolved, nitrogen protection
Under, 80~85 DEG C of 18~20h of reaction, prepolymer P is obtained, wherein above-mentioned hydrophilic modifier, surface fixative, initiator and phosphoric acid
The mass ratio of triethyl is 7~8:5~6:0.1~0.2:180~220；
(2) by above-mentioned prepolymer P and deionized water with volume ratio 1~1.5:1 is well mixed to obtain modified solution；
(3) above-mentioned doughnut cladding adsorptive resin is immersed in above-mentioned modified solution, stirring 1.5~2.0h of immersion, directly
Adsorptive resin microswelling is coated to doughnut；
(4) doughnut of microswelling cladding adsorptive resin is taken out from modified solution, be dipped to again concentration for 1.0~
In 1.5wt.% citric acid solution, 8~10h of hydrolysis process at 55~60 DEG C；
(5) the doughnut cladding adsorptive resin after lemon acid soak is put into physiological saline, soaks 3~4d, dry
Required compound doughnut polymeric adsorbent is obtained after sterilizing.
3. preparation method as claimed in claim 1, it is characterised in that the macroreticular resin is porous poly- micro- to benzene divinyl
Ball.
4. preparation method as claimed in claim 3, it is characterised in that the macroreticular resin be XT30 or fpa 90ci in extremely
Few one kind.
5. preparation method as claimed in claim 1, it is characterised in that the condition of sonic oscillation processing is：Ultrasonic wave frequency
Rate is 40~50KHz, and temperature is 25~30 DEG C.
6. preparation method as claimed in claim 1, it is characterised in that the preparation method of the polysulfones particle in the step (4)
For：By polysulfones grain dissolution in organic solvent, 20~25h is stirred under the conditions of 75~80 DEG C, polysulfones solution is obtained, wherein above-mentioned
The mass ratio of polysulfones particle and organic solvent is 1:4~5, above-mentioned organic solvent is 1-METHYLPYRROLIDONE, dimethyl acetamide
Or one kind in N,N-dimethylformamide.
7. preparation method as claimed in claim 2, it is characterised in that in the hydrophilic modifier containing pyrrolidone group and
Carbon-carbon double bond group.
8. preparation method as claimed in claim 7, it is characterised in that the hydrophilic modifier is vinyl pyrrolidone.
9. preparation method as claimed in claim 2, it is characterised in that in the surface fixative containing carbon-carbon double bond group and
Ethoxysilane groups, or contain carbon-carbon double bond group and methoxy silane groups.
10. preparation method as claimed in claim 9, it is characterised in that the surface fixative is vinyl triethoxyl silicon
At least one of alkane or vinyltrimethoxy silane.
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