CN104174385B - A kind of adsorbent for bilirubin for blood perfusion - Google Patents
A kind of adsorbent for bilirubin for blood perfusion Download PDFInfo
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- CN104174385B CN104174385B CN201410362280.0A CN201410362280A CN104174385B CN 104174385 B CN104174385 B CN 104174385B CN 201410362280 A CN201410362280 A CN 201410362280A CN 104174385 B CN104174385 B CN 104174385B
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Abstract
A kind of adsorbent for bilirubin for blood perfusion .Present invention principle based on molecular engram, with the oligomeric big molecule with human serum albumins with similar molecular weight etc. as pore-foaming agent, with polystyrene-divinylbenzene as basic framework,By free radical suspensioning polymerization methodIt is prepared for the adsorbent of ultra-large aperture high-specific surface area.This adsorbent not only has the specific surface area of superelevation, it may have be suitable for the duct of A-bB free diffusing, all has good adsorption effect to combining with unconjugated bilirubin.Meanwhile, the features such as this invention adsorbent, than tradition adsorbent for bilirubin, also has preparation technology simple, good biocompatibility, and adsorption capacity is big, electroless matter disorder risk, cannot be only used for plasma perfusion it can also be used to whole blood perfusion removes bilirubin.
Description
Technical field
The invention belongs to biomedicine technical field, relate to the Medical Adsorbents of a kind of novelty, be particularly suitable for passing through
Extracorporeal blood perfusion removes too high bilirubin and the adsorbent of cholic acid in blood.
Background technology
Bilirubin (Bilirubin BR) is one of primary pigments of bile, red blood cell aging produce, mainly through liver
Drain after metabolism.As internal bilirubin produces too much, or liver is to bilirubinic picked-up, metabolism or excretory function generation obstacle,
Bilirubin will be accumulated in vivo, causes Bilirubinemia.Unconjugated bilirubin is a kind of endogenous toxin, and its lipophilicity is
It is easily by biomembrane, and deposits in tissue, causes the xanthochromia such as sclera, skin.When unconjugated bilirubin concentration in blood plasma
During more than 20-25mg/dl, its permeable blood brain barrier and nerve nucleus combine, and disturb function of brain cell, cause brain not
Reversible damage, i.e. bilirubin encephalopathic, prognosis is very poor, even jeopardizes patient vitals.It addition, a lot of diseases are all red with courage clinically
Element savings in vivo is relevant, if the bilirubin of excess in the patient can effectively be removed, for improving quality of life, saving and suffer from
Person's life is significant.
Treatment to hyperbilirubinemia mainly uses phototherapy, drug therapy, plasma exchange and blood clean the most clinically
Change (dialysis and blood perfusion etc.) treatment etc..Phototherapy is mainly for the lighter patient of symptom；Drug therapy clinical effect is the most highly desirable,
Patients symptomatic tends not to be improved in time；Plasma exchange needs a large amount of fresh plasmas, costly and limited source, and
There is cross-infection risk；Haemodialysis has better effects to little molecule, soluble toxins, to fat-soluble bilirubin and pay no attention to
Think；For bilirubinic removing, blood perfusion has a clear superiority, and obtains clinic and increasingly focus on.
In terms of the hemoperfusion treatment of hyperbilirubinemia, the sorbent material used is mainly activated carbon and synthesis
Resin.Activated carbon specific surface area is high, average pore size is less, not ideal to bilirubinic adsorption effect, and easily retting conditions draws
Play embolism.The application of synthetic resin then focuses primarily upon macroporous type anion exchange resin field, as Kuraray company of Japan is raw
The BL-300 produced, the BR-350 of Asahi Chemical Industry of Japan, the MARS system of Germany, the product such as the BS-300 of China's key sail is sorbent used
Being resin anion (R.A.), these resins, because with strong basicity group, using plasma perfusion modes more, have simultaneously and cause blood electricity
Solve the risk that matter is disorderly.In research field, there is employing styrene carrier, be aglucon by activated grafting active amino, dextrin etc.；
Employing polyvinyl alcohol is carrier, is grafted polyamines aglucon；Using agarose carrier, being grafted the molecule with amido is aglucon；Also have
Introducing the polymeric adsorbent of cyano group etc. in styrene skeleton, above resin, based on many factors, remains in laboratory research, grinds
Study carefully data also many removings based on little molecule unconjugated bilirubin, so the reality that clinical practice is faced can not truly be reflected.
At present in terms of the research of adsorbent for bilirubin, be still lipophilicity segment based on bilirubin molecular structure and bear from
Sub-carboxyl, increases the elimination effect to blood mesobilirubin by introducing cation amido on the sorbent.But such adsorbent
Being simply possible to use in plasma perfusion, and biocompatibility is poor, there is the problems such as electrolyte disturbance needs to pay close attention to, and is also greatly increased simultaneously
The medical expense of patient.
China does not the most still have one to may be used for whole blood perfusion, and the adsorbent product to bilirubin elimination effect excellence
Occur.Therefore, a kind of novel adsorbent for bilirubin product of urgent clinical needs, it can be used not only for whole blood perfusion, and can high-efficient cleaning
Except the bilirubin in blood, also there is the cost of relative moderate simultaneously, make blood perfusion technique more wide range of services in extensive patients.
Summary of the invention
The present invention seeks to the deficiency existed for existing adsorbent for bilirubin, it is provided that a kind of good biocompatibility, intensity
High, adsorption capacity big and low cost of manufacture, adsorbent for bilirubin that can be used for whole blood perfusion and preparation method thereof.
What the present invention provided obtains adsorbent for bilirubin for blood perfusion, is with crosslinked polystyrene-divinylbenzene microspheres
For underlying carrier, with oligomeric macromolecule (low polystyrene of degree of polymerization 100-1000, the oligomeric methyl third of degree of polymerization 100-1000
Olefin(e) acid esters, the polyvinyl acetate etc. of degree of polymerization 200-800), toluene, liquid wax, solid wax and their scalemic thereof be
Pore-foaming agent, the macroporous absorbent resin microballoon prepared by free radical suspensioning polymerization method, then this microballoon is used and there is good biological
Compatibility material carries out coating, improves biocompatibility and the adsorptive selectivity of adsorbent further；
Carrier is spherical, and swellbility is low, and mechanical strength is good, particle diameter between 0.3-1.0mm, specific surface area 500-
1500m2/ g, aperture 5-50nm.
The present invention preferentially selects styrene-divinylbenzene polymer microballoon to be carrier material, this material preparation process is simple,
Structure can flexible modulation.
The coated fertilizer that the present invention selects is collodion or poly hydroxy ethyl acrylate.By regulation coated fertilizer
Thickness, while increasing carrier good biocompatibility, it is possible to gives the inhaling the selectivity of material in blood of adsorbing agent carrier
Attached effect.Coated fertilizer used is alternatively shitosan, heparin, polyvinyl alcohol, heparin etc..
The adsorbent that the present invention provides can be used for plasma perfusion and removes bilirubin, or for whole blood perfusion.
The preparation method of the adsorbent that the present invention provides, can be realized by following steps:
Prepared by the 1st step, crosslinked polystyrene-divinylbenzene macroporous microsphere
1.1st, at normal temperatures, gelatin or polyvinyl alcohol are dissolved in the water, are made into 1.0-2.0%(mass fraction) water
Phase, is heated to 30-55 DEG C so that gelatin or polyvinyl alcohol fully dissolve；
1.2nd, styrene with mass ratio as 0-1:1 and divinylbenzene are as reaction monomers；With reaction monomers 0.5-3 times
The low polystyrene of (mass ratio), oligomeric methacrylate class, polyvinyl acetate, toluene, liquid wax, solid wax etc., or they
Scalemic thereof be pore-foaming agent；Reaction monomers and pore-foaming agent are mixed, referred to as oil phase.
1.3rd, being mixed with oil phase by above-described aqueous phase, wherein aqueous phase is 3-4:1 with the volume ratio of oil phase；With peroxide
Changing benzoyl or azo-bis-isobutyl cyanide is initiator, consumption is the 1-3% of mix monomer gross mass；Through suspension polymerisation, with 1-2 DEG C/
The speed of 5 minutes is to slowly warm up to 70-80 DEG C, reacts 3-5 hour, then is to slowly warm up to 85 DEG C with the speed of 1-2 DEG C/5 minutes
Reacting 3-5 hour, then be to slowly warm up to more than 95 DEG C with the speed of 1-2 DEG C/5 minutes, react 3-5 hour, reaction system is passed through
After filter, carrying out washing treatment, prepare polystyrene macropore ball, standby.
2nd step, coating
2.1st, coating agent (collodion or poly hydroxy ethyl acrylate etc.) is dissolved in solvent (ethanol, ether etc. or it
Mixed solvent) in, prepare concentration be 0.1-1%(coating agent and solvent quality than) coating agent solution.
2.2nd, then take adsorbent prepared by the 1st step, coating agent solution is joined in adsorbent, make adsorbent obtain
Fully soaking, coating agent consumption is 1-3 times (volume ratio) of adsorbent.Fully clean by ethanol or deionized water again, wrapped
The adsorbent product of film.
The outward appearance of adsorbent for bilirubin prepared by the present invention and physical and chemical parameter be: milky spheric granules, particle diameter 0.3-
1.0mm, specific surface area 500-1500m2/ g dried resin, water content 50-65%, average pore size 5-50nm, porosity 50-80%.Should
Adsorbent can be used for blood perfusion and removes the bilirubin in blood.
Advantages of the present invention and beneficial effect
The present invention, according to the bilirubinic molecular size of albumin-binding, devises large aperture, high-specific surface area polyphenyl second
Ene-type adsorbent.By kind and the thickness of regulation coated fertilizer, while being possible not only to increase carrier good biocompatibility,
Also can give adsorbing agent carrier to the selective absorption effect of material in blood.Adsorption experiment shows, the bilirubin of the present invention
Adsorbent has excellent absorption property and blood compatibility to the bilirubin in blood, is used for treating hyperbilirubinemia peace
Entirely, effectively.
Accompanying drawing explanation
Fig. 1 is that different adsorbent is to bilirubinic adsorption rate test result figure.
Detailed description of the invention
The preparation of embodiment 1 high Crosslinked Macroporous microballoon
At normal temperatures, by 10g Gelatin in 1000ml water, be made into 1.0%(mass fraction) the aqueous solution, be placed in
The there-necked flask of 2000ml is heated to 45 DEG C so that gelatin fully dissolves；By 50g styrene, 100g divinylbenzene, 110g first
Benzene, 190g atoleine, 10g low polystyrene (degree of polymerization 1000) and 1.5g azo-bis-isobutyl cyanide add three after mixing
In mouth bottle, starting stirring, regulation rotating speed makes oil droplet be dispersed into modest size, through suspension polymerisation, delays with the speed of 1-2 DEG C/5 minutes
Slowly it is warming up to 78 DEG C, reacts 3 hours, then be to slowly warm up to 85 DEG C with the speed of 1-2 DEG C/5 minutes, react 3 hours, then with 1-2
DEG C/speed of 5 minutes is to slowly warm up to more than 95 DEG C, reacts 5 hours, then stops reaction, filter, after carrying out washing treatment, preparation
Go out crosslinked polystyrene-divinylbenzene macropore ball.Particle diameter 0.5-1.0mm, average pore size 25nm, specific surface area 620m2/g。
The preparation of embodiment 2 high Crosslinked Macroporous microballoon
At normal temperatures, 18g polyvinyl alcohol is dissolved in 1200ml water, is made into 1.5%(mass fraction) the aqueous solution, put
45 DEG C it are heated to so that polyvinyl alcohol fully dissolves in the there-necked flask of 3000ml；By styrene 25g, 125g divinylbenzene,
20g oligomeric methacrylate class, 80g toluene, 25g atoleine, 25g solid paraffin and the mixing of 2.0g benzoyl peroxide are all
Adding in there-necked flask after even, start stirring, regulation rotating speed makes oil droplet disperse, through suspension polymerisation, with the speed of 1-2 DEG C/5 minutes
It is to slowly warm up to 78 DEG C, reacts 3 hours, then be to slowly warm up to 85 DEG C with the speed of 1-2 DEG C/5 minutes, react 3 hours, then with 1-
The speed of 2 DEG C/5 minutes is to slowly warm up to more than 95 DEG C, reacts 5 hours, then stops reaction, after filtration, carrying out washing treatment, and preparation
Go out high crosslinked polystyrene-divinylbenzene macropore ball.Particle diameter 0.3-1.0mm, average pore size 25nm, specific surface area 700m2/g。
The preparation of embodiment 3 high crosslinking super big hole microballoon
At normal temperatures, 20g polyvinyl alcohol is dissolved in 1000ml water, is made into 2.0%(mass fraction) the aqueous solution, put
45 DEG C it are heated to so that polyvinyl alcohol fully dissolves in the there-necked flask of 2000ml；By 150g divinylbenzene, 200g toluene,
190g solid paraffin, 15g polyvinyl acetate (degree of polymerization 500) and 1.5g benzoyl peroxide add three mouthfuls after mixing
In Ping, starting stirring, regulation rotating speed makes oil droplet be dispersed into modest size, through suspension polymerisation, slow with the speed of 1-2 DEG C/5 minutes
Be warming up to 78 DEG C, react 3 hours, then be to slowly warm up to 85 DEG C with the speed of 1-2 DEG C/5 minutes, react 3 hours, then with 1-2 DEG C/
The speed of 5 minutes is to slowly warm up to more than 95 DEG C, reacts 5 hours, then stops reaction, after filtration, carrying out washing treatment, prepares height
Crosslinking super big hole microballoon.Particle diameter 0.3-1.0mm, average pore size 45nm, specific surface area 1200m2/g。
Embodiment 4 collodion coating
Accurately weigh the microballoon 10ml handled well in embodiment 1, under stirring, join 10ml mass ratio Han 1%() collodion
Ethanol solution in, continue stirring, make collodion be uniformly distributed in microsphere surface, after reclaiming alcohol solvent, by resin after coating
After repeatedly rinsing with water for injection, drying for standby, numbering: SSL-1.
Embodiment 5 coating
By the hydroxyethyl methacrylate polymer of 0.5% degree of cross linking of 0.1g, it is dissolved in the ether of 20ml, prepares
To the coating agent solution of 0.5%, the most accurately weigh the microballoon 10ml handled well in embodiment 2, join ether under stirring molten
In liquid, continue stirring, make poly hydroxy ethyl acrylate polymer uniform be distributed in microsphere surface, after reclaiming ether solvent, will
After after coating, resin water for injection rinses repeatedly, drying for standby, numbering: SSL-2.
Embodiment 6 coating
By the hydroxyethyl methacrylate polymer of 0.5% degree of cross linking of 0.02g, it is dissolved in the ether of 20ml, prepares
To the coating agent solution of 0.1%, the most accurately weigh the microballoon 10ml handled well in embodiment 3, join ether under stirring molten
In liquid, continue stirring, make hydroxyethyl methacrylate polymer uniform be distributed in microsphere surface, after reclaiming ether solvent, will bag
After after film, resin water for injection rinses repeatedly, drying for standby, numbering: SSL-3.
Embodiment 7 macroporous microsphere Staticadsorption experiment
The preparation that simulation hyperbilirubinemia is asked: weigh 2.0g bovine serum albumin(BSA), adds PBS 133ml and dissolves,
To simulation serum solution.The most accurately weigh 15mg bilirubin, with 3.0ml dimethyl sulfoxide and 2.0ml sodium carbonate liquor (0.l mol/L)
Dissolve, and with the simulation serum solution constant volume joined, obtain the bilirubin solution of 100ml.
SSL-1, SSL-2, SSL-3 macroporous microsphere in Example 4,5,6 is test group, with XAD-4(U.S. Luo Menha
This company buys) resin is comparative study object, takes various types of resins 0.5ml respectively in 25ml conical flask, with syringe by water
Blot, add 15ml and simulate hyperbilirubinemia clear liquid, stopper with stopper, and seal with sealed membrane.Lucifuge is placed in air table,
37 DEG C of concussion absorption 2h.
Taking supernatant and survey bilirubin concentration, and set blank, often group test is in triplicate, and calculates suction according to following equation
Attached amount and the adsorption rate of unit volume resin:
AP=
In formula, AP is adsorption rate (%),WithIt is respectively bilirubinic concentration (mg/dl) before and after absorption.
Test result is for being shown in Fig. 1, and result is visible, XAD-4 to simulation serum in bilirubinic adsorption rate about 40%,
And resin of the present invention to the bilirubinic adsorption rate in same system all more than 85%, exceed more than one times than control group.
Embodiment 8 macroporous microsphere static state blood compatibility is tested
Weigh 0.2mL adsorbent SSL-1, SSL-2, SSL-3 respectively, join after fully rinsing with sodium chloride injection
In the human blood of 2mLEDTA-K2 anti-freezing, being not added with adsorbent in blank group blood, 2h is placed in 37 DEG C of water-baths, takes 20 l respectively
The change of haemocyte index is measured in blood cell analyzer.
Result see table:
From table, result understands: the adsorbent of gained of the present invention, is respectively provided with good blood compatibility.
Claims (3)
1. the adsorbent for bilirubin for blood perfusion, it is characterised in that this adsorbent is with polystyrene-divinylbenzene
For carrier, this carrier is with toluene, liquid wax, solid paraffin, oligomeric macromolecule and their scalemic thereof as pore-foaming agent, presses
The macroporous absorbent resin microballoon that free radical suspensioning polymerization method prepares, then uses this microballoon and has good biocompatibility
Material carries out coating, improves the biocompatibility of adsorbent further；Described oligomeric macromolecule pore-foaming agent is degree of polymerization 100-
The low polystyrene of 1000, the polyvinyl acetate of degree of polymerization 200-800 and the polymethacrylates of degree of polymerization 100-1000,
Coated fertilizer used is collodion or cross-linked poly-methyl methacrylate β hydroxyl ethyl ester.
Adsorbent the most according to claim 1, it is characterised in that between described microspherulite diameter 0.3-1.0mm, specific surface
Long-pending 500-1500m2/ g, aperture 5-50nm.
3. the application of the adsorbent described in claim 1, removes bilirubin for plasma perfusion, or for whole blood perfusion.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104624170B (en) * | 2014-12-25 | 2017-02-01 | 佛山市博新生物科技有限公司 | Adsorbent for treating gram bacterial infection and blood perfusion device |
| CN105126785A (en) * | 2015-07-31 | 2015-12-09 | 珠海健帆生物科技股份有限公司 | Adsorbent, preparation method thereof, and resin containing long-chain quaternary ammonium salt |
| CN107262057B (en) * | 2016-04-08 | 2020-04-17 | 中国科学院大连化学物理研究所 | Preparation method of bilirubin anion resin adsorbent |
| CN106238016B (en) * | 2016-09-13 | 2019-01-11 | 苏州驿通滤材科技有限公司 | A kind of bilirubin removal preparation method of blood perfusion resin sorbent |
| CN106622169B (en) * | 2016-12-14 | 2019-07-12 | 广州市恩德氏医疗制品实业有限公司 | A kind of Medical Adsorbents and its preparation method and application |
| CN109513429A (en) * | 2017-09-18 | 2019-03-26 | 重庆希尔康血液净化器材研发有限公司 | A kind of preparation method of modified adsorbent for bilirubin |
| CN114106406A (en) * | 2020-08-31 | 2022-03-01 | 泉州师范学院 | Ultrahigh cross-linked porous resin adsorbent for blood perfusion and preparation method thereof |
| CN112221474B (en) * | 2020-09-23 | 2023-04-07 | 重庆天外天生物技术有限公司 | Bilirubin adsorbent with high mechanical strength and good biocompatibility and preparation method thereof |
| CN113262762B (en) * | 2021-05-06 | 2023-04-21 | 西安蓝深新材料科技股份有限公司 | Adsorption material for blood perfusion and preparation method thereof |
| CN113372474B (en) * | 2021-06-29 | 2023-10-20 | 西安蓝晓科技新材料股份有限公司 | Blood perfusion resin and preparation method and application thereof |
| CN114950383B (en) * | 2022-04-08 | 2024-02-06 | 淄博康贝医疗器械有限公司 | Cytokine adsorbent for blood purification and preparation method thereof |
| CN115746200B (en) * | 2022-10-21 | 2024-01-26 | 四川大学 | Gel microsphere capable of adsorbing and decomposing bilirubin, preparation method and application thereof |
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| CN1289183C (en) * | 2004-01-30 | 2006-12-13 | 浙江科锐生物科技有限公司 | Method for preparing macromolecule resin type bilirubin sorbent |
| CN101357963A (en) * | 2007-08-01 | 2009-02-04 | 中国科学院大连化学物理研究所 | Preparation method of polystyrene-divinylbenzene microspheres for bilirubin adsorption |
| CN101612543A (en) * | 2008-06-25 | 2009-12-30 | 中国科学院大连化学物理研究所 | Be used for the preparation of the polystyrene-divinylbenzene microspheres of blood purification |
| CN102847521B (en) * | 2011-06-28 | 2013-07-10 | 于杰 | Macro-porous adsorption resin and its application |
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Effective date of registration: 20180428 Address after: 300457 Tianjin Development Zone, two street, two street, A District, No. 9 Patentee after: Tianjin Younasi Biotechnology Co., Ltd. Address before: No. 94 Wei Jin Road, Nankai District, Tianjin Patentee before: Nankai University |