CN102746440B - Preparation technology of polystyrene microsphere for reinforcing turbidimetric reagent - Google Patents
Preparation technology of polystyrene microsphere for reinforcing turbidimetric reagent Download PDFInfo
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- CN102746440B CN102746440B CN 201210276627 CN201210276627A CN102746440B CN 102746440 B CN102746440 B CN 102746440B CN 201210276627 CN201210276627 CN 201210276627 CN 201210276627 A CN201210276627 A CN 201210276627A CN 102746440 B CN102746440 B CN 102746440B
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Abstract
The invention relates to a preparation technology of a polystyrene microsphere for reinforcing a turbidimetric reagent. A reaction system of the preparation technology comprises an external water phase, a polymeric monomer and a functional monomer, wherein the external water phase comprises 0.1-2g of sodium dodecyl sulfate, 2-16g of polyethylene glycol 6000, 0.1-3g of sodium chloride and 400-600mL of purified water; the polymeric monomer comprises 50-100mL of styrene and 0.5-1.0mL of divinyl benzene; and the functional monomer comprises 2-16mL of ethyl acrylate and 10-60mL of a boric acid andborax buffer solution. Carboxylated polystyrene microsphere is obtained through configuration of the external water phase, purification of the polymeric monomer and preparation and polymerization reaction of an emulsion. According to the polystyrene microsphere produced through the preparation technology, the cost is 1% of the price of microspheres in foreign companies, the anti-agglutination effect is more than ten times better than that of the microspheres in foreign companies, the cross-linking efficiency with antibodies is improved by 50%, and the multi-purpose microsphere can satisfy requirements of a plurality of projects.
Description
Technical field
Field of polymer microsphere materials of the present invention particularly, relates to a kind of preparation technology who is applied to strengthen than the polystyrene microsphere of turbid reagent.
Background technology
The preparation and application aspect development of polystyrene microsphere is very fast, not only many new technologies have been developed on the basis of traditional letex polymerization and suspension polymerization, also perfect day by day on the performance of microballoon, kind, progressively develop into can synthesize that single dispersion, particle diameter are controlled, variform, structure, high performance product, be widely used in fields such as standard metering, food chemical industry, medicine and pharmacology, biotechnology, information engineering and microelectronics, particularly be applied in biomedical sector, significant to the research of clinical diagnosis, check, immunological technique, cytology etc.In the external diagnosis reagent industry, polystyrene microsphere is to strengthen one of important source material than turbid reagent, and the performance of microballoon has determined the performance of reagent.
Letex polymerization (emulsion polymerization) is a kind of synthetic method commonly used in the Polymer Synthesizing process, and is because it is with water as solvent, very favourable to environment.Under the effect of emulsifying agent and by means of mechanical stirring, make monomer in water, be dispersed into milk sap, the polyreaction of being undertaken by the initiator initiation.Though being collectively referred to as method, this has developed decades, but because moiety is more in synthetic, each material proportion complexity, really can be advantageously applied to now enhancing than the polystyrene microsphere of turbid reagent seldom, the microballoon that performance is more stable also mainly comes from external major company, and is expensive, as Polymicrospheres, Bangslabs etc., expensive, be that 300 RMB-600 RMB/g do not wait.And the polystyrene microsphere of many homemade producers exists difference between batch big, poor stability, problem such as application performance is bad.These problems of existing polystyrene microsphere also are that many domestic manufacturers do not strengthen than one of the research and development of turbid reagent and major reason of throughput.
Polystyrene microsphere uses the microballoon of offshore company will cause other raw material of producing reagent to increase as strengthening one of important source material than turbid reagent, and reagent cost raises.Simultaneously, the microballoon of offshore company a lot of problems also occurred in than the process of turbid reagent being applied to enhancing, and on the low side as easy cohesion and antibody linked efficient, the production efficiency of reagent is difficult to problems such as raising.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation technology who is applied to strengthen than the polystyrene microsphere of turbid reagent.
The present invention solves the problems of the technologies described above the technical scheme that adopts: a kind of preparation technology who is applied to strengthen than the polystyrene microsphere of turbid reagent, reaction system comprises outer water, polymerization single polymerization monomer and function monomer, and the component of described outer water and content are: sodium lauryl sulphate 0.1-2g, polyethylene glycol 6000 2-16g, sodium-chlor 0.1-3g, purified water 400-600mL; The component of polymerization single polymerization monomer and content are: vinylbenzene 50-100mL, Vinylstyrene 0.5-1.0 mL; The component of function monomer and content are: ethyl propenoate 2-16mL, boric acid borate buffer solution 10-60mL; This preparation technology comprises the steps:
(1) configuration of outer water: accurately measure purified water according to the content ratio of outer water and place dissolution vessel, accurately take by weighing sodium lauryl sulphate, polyethylene glycol 6000 and sodium-chlor again in dissolution vessel, stirring and dissolving;
(2) purifying of polymerization single polymerization monomer: by measuring vinylbenzene and Vinylstyrene containing of polymerization single polymerization monomer in separating funnel, add sodium hydroxide solution and shake up, the stopper in the desolventizing is drawn unnecessary sodium hydroxide with purified water then;
(3) preparation of emulsion: stir the outer water for preparing and simultaneously the polymerization single polymerization monomer behind the purifying slowly is added dropwise to the outer aqueous phase for preparing, drip the mixing back and with ultrasonic instrument is ultrasonic it is uniformly dispersed;
(4) polyreaction: finely dispersed emulsion is poured in the reaction vessel, stirring heating, after treating that temperature rises to 65-85 ℃, add the initiator initiation reaction, after reaction 30-60min generates the polystyrene microsphere of no function group, add function monomer, reacted 5.5-7.5 hour, obtain carboxylic polystyrene microsphere.
Particularly, the rotating speed that stirs in the described step (1) is 500-800rpm.
The quality percentage composition of sodium hydroxide solution is 5% in the described step (2).
The rotating speed that stirs in the described step (3) is 600rpm.
The power 40khz of ultrasonic instrument in the described step (3), ultrasonic to make the time of its dispersion be 10-30min.
Initiator in the described step (4) is ammonium persulphate.
Function monomer divides 2 to 4 addings in the described step (4), and the amount that at every turn adds function monomer equates.Be about to divide n adding after function monomer evenly is divided into n part.N=2 or 3 or 4.
As adding mode preferably, function monomer divides 4 addings in the described step (4).
Described function monomer is that ethyl propenoate is scattered in the solution that the boric acid borate buffer solution constitutes.
The polystyrene microsphere that application performance is superior, it mainly is subjected to composition of raw materials and two big factor affecting of technical process, and the core technology of technique scheme of the present invention is also just aspect these two.On original letex polymerization basis, increased the assistant for emulsifying agent polyoxyethylene glycol, make the microballoon of preparation Paint Gloss, size distribution is narrower; And added the adjusting material (sodium-chlor) of ionic strength, and be beneficial to charge balance, be conducive to the stability of whole emulsion system, the phenomenon of breakdown of emulsion can not appear.On polymer monomer, added linking agent (Vinylstyrene), make the polystyrene microsphere structure that obtains finer and close, molecular weight is higher.In the dispersion system of function monomer, added the boric acid borate buffer solution innovatively, regulated the acidity of whole system effectively, production technique is very stable.
Further, acting in conjunction by temperature and stirring velocity, we can accurately control the size (deviation is no more than 10 nm) of the polystyrene microsphere that is synthesized, the mode that adds function monomer by needle tubing has solved the excessive problem of local acidity in the emulsion of function monomer adding back, and stability of emulsion is fine.
Among the above-mentioned preparation technology of the present invention, step (2) is the purifying of polymerization single polymerization monomer, according to the usage of trade and requirement, the vinylbenzene of producing and Vinylstyrene all can add stopper when preserving, stopper can select Resorcinol HQ(to have another name called quinhydrones, and the most frequently used, price is low.The normal temperature effect is better; the heating cure effect is relatively poor) or para benzoquinone PBQ(under anoxia condition, still can play a role; be applicable to the etherification procedure color Huang of nitrogen or other protection of inert gas; influential to color of resin) or toluhydroquinone THQ(effective; be used for the production of high reactivity unsaturated polyester resin, be usually used in gel coating resin, SMC resin.This product solvability is good, and the high temperature polymerization inhibition effect is good), for fear of the influence of stopper to technology of the present invention, it is that 5% sodium hydroxide solution is removed stopper that the present invention adopts massfraction, certainly, also can adjust the content of sodium hydroxide in the sodium hydroxide solution as the case may be.Ultrasonic instrument in the step (3) can select for use promotion commonly used such as ultrasonator to dissolve finely dispersed ultrasonic device.
Compared with prior art, the invention has the beneficial effects as follows:
1, the polystyrene microsphere that adopts preparation technology of the present invention to produce, cost is 1% of offshore company's microballoon price.
2, the polystyrene microsphere that adopts preparation technology of the present invention to produce is with short production cycle, a complete set of production technique only 6 hours consuming time.
3, adopt polystyrene microsphere that preparation technology of the present invention produces on using and superior, anti-freezing collection effect is that tens times of offshore company's microballoon and the cross-linking efficiency of antibody have improved 50%.
4, behind the polystyrene microsphere that employing preparation technology of the present invention produces, enhancing is to use 2 times of offshore company's microballoon than turbid reagent production efficiency.
5, adopt the polystyrene microsphere that preparation technology of the present invention produces after, strengthen than the cost of turbid reagent and descended 40% when using offshore company's microballoon.
6, the polystyrene microsphere that adopts preparation technology of the present invention to produce can reach the requirement that a kind of microballoon satisfies a plurality of projects simultaneously, and a ball is used more.
Description of drawings
Fig. 1 is synthesis process flow diagram of the present invention;
Fig. 2 is the experimental result picture of polystyrene microsphere in the application of a1-MG mensuration test kit of example 1 preparation;
Fig. 3 is the experimental result picture of polystyrene microsphere in the application of retinol conjugated protein mensuration test kit of example 1 preparation;
Fig. 4 is the experimental result picture of polystyrene microsphere in the application of bladder chalone C determining reagent kit of example 2 preparations;
Fig. 5 is the experimental result picture of polystyrene microsphere in the application of B2-MG mensuration test kit of example 2 preparations;
Fig. 6 is the experimental result picture of polystyrene microsphere in the application of myohaemoglobin mensuration test kit of example 3 preparations.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, but embodiments of the present invention are not limited only to following embodiment.
Being applied to of present embodiment strengthens among the preparation technology than the polystyrene microsphere of turbid reagent, and core technology is embodied in composition of raw materials and two aspects of technical process.
The composition of raw materials material proportion is as follows:
Outer water: sodium lauryl sulphate (SDS) 0.1-2 g; Polyoxyethylene glycol (PEG-6000), namely molecular weight is 6000 polyoxyethylene glycol 2-16 g; Sodium-chlor (NaCl) 0.1-3 g; Purified water (H
2O) 400-600 mL.
Polymerization single polymerization monomer: vinylbenzene (St) 50-100 mL; Vinylstyrene (DVB) 0.5-1.0 mL.
Function monomer: ethyl propenoate 2-16 mL, boric acid borate buffer solution 10-60 mL.
Said ratio as the present invention's prescription can zoom in or out according to its ratio geometric ratio.The reaction vessel of its reaction process and the specification of relevant device, also adjustment and the design that adapts according to how much making of reactant.
The concrete prescription of present embodiment is as shown in table 1:
Table 1
| Synthesizing formula | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Sodium lauryl sulphate | 2g | 1g | 0.1g | |
| Polyoxyethylene glycol (6000) | 16g | 8g | 2g | |
| Sodium-chlor | 0.1g | 1.5g | 3g | |
| Vinylbenzene | 10mL | 75mL | 50mL | |
| Vinylstyrene | 1mL | 0.75mL | 0.5mL | |
| Ethyl propenoate | 16mL | 8mL | 2mL | |
| The boric acid borate buffer solution | 60mL | 35mL | 10mL | |
| Ultrapure water | 600mL | 500mL | 400mL | |
| Synthesis technique | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Temperature | 85℃ | 75℃ | 65℃ | |
| Stirring velocity | 800rpm | 650?rpm | 500?rpm | |
| | 30min | 20? |
10?min | |
| Add the function monomer number of times | 4 | 1 | 1 | |
| The function monomer ratio | 1∶1∶1∶1 | / | / | |
| Reaction times | 8h | 7h | 6h | |
| Cost (RMB/g) | 2.35 | 3.15 | 3.65 |
Technical process comprises the steps:
(1) preparation of outer water
Accurately measure an amount of purified water in beaker according to the ratio of formula table, accurately take by weighing sodium lauryl sulphate (SDS), polyoxyethylene glycol (PEG-6000) and sodium-chlor again in beaker, 500-800rpm rotating speed stirring and dissolving.
(2) purifying of polymerization single polymerization monomer
Measure vinylbenzene and Vinylstyrene in proportion in separating funnel, add certain density sodium hydroxide and shake up, the stopper in the desolventizing.Draw unnecessary sodium hydroxide with purified water at last.
(3) preparation of emulsion
The polymerization single polymerization monomer good purifying slowly is added dropwise to the outer aqueous phase for preparing under the water 600rpm rotating speed outside.Mixing the back is uniformly dispersed it with ultrasonic instrument ultrasonic (power 40khz) 10-30min.
(4) polyreaction
Scattered emulsion is poured in the reaction vessel of appointment, stirring heating, after treating that temperature rises to assigned temperature, adding the initiator ammonium persulfate initiation reacts, after the polystyrene microsphere of no function group generates after reaction for some time, add function monomer (ethyl propenoate) solution (adding respectively for 1 to 4 time by a certain percentage) for preparing in advance, be reacted to the scheduled time (6-8 hour), namely generate carboxylic polystyrene microsphere.
Function monomer is that ethyl propenoate is scattered in the solution that the boric acid borate buffer solution constitutes.
Adopt above-mentioned prescription and synthesis technique, reacted material is measured through laser particle size analyzer and potentiometric titrator, and product is carboxylic polystyrene microsphere.
In the table 1, temperature in the synthesis technologic parameter is the temperature that rises to reaction in the step (4), stirring velocity is the rotating speed of stirring and dissolving in the step (1), cost is according to the prescription of present embodiment and technical process, by the input of material with finally obtain the production cost of every gram carboxylic polystyrene microsphere that the amount of product carboxylic polystyrene microsphere calculates.Find that through overtesting under the identical situation of other test conditionss, its cost had tangible reduction with respect to once adding when the number of times of adding function monomer was 2-4 time.Dividing under the situation about adding for 4 times, with respect to 1 adding, its cost significantly reduces.
For prescription and the prepared carboxylic polystyrene microsphere of synthesis technique pressed in above-described embodiment in the table 1, we carry out further experiment.
Table 2
According to the experimental result of table 2, carboxylic polystyrene microsphere is as a kind of raw material for the production of other reagent, and the carboxylic polystyrene microsphere cost of present embodiment is for external microballoon, and cost only is 1% of offshore company's microballoon price.External microballoon in the table 2 is the polymicrospheres microballoon.The polymicrospheres microballoon is a kind of in the existing microballoon of offshore company.
In table 1, press component and the prepared carboxylic polystyrene microsphere of technology of embodiment 1-3 for present embodiment, carry out application experiment respectively, in the application experiment below, for the contrast experiment in the same table, adopt microballoon to prepare ratio, parameter and the method for reagent, except microballoon different, other component is all identical with condition, and the method that adopts microballoon to make reagent is existing technology, and those skilled in the art adopt conventional reagent compounding process to realize.
These microballoons are as shown in the table (in following each table in the relevant experimental data of the application of preparation related reagent, all data are all measured by automatic clinical chemistry analyzer, location parameter and measuring method are prior art, and those skilled in the art adopt conventional determination techniques to realize.
Table 3
| A1-MG calibration object concentration (mg/L) | Embodiment 1 | The CB096D microballoon of polymicrospheres |
| 0 | -19 | -77 |
| 14 | 1004 | 602 |
| 28 | 2312 | 1284 |
| 49 | 4277 | 2097 |
| 98 | 8222 | 3022 |
| 140 | 9892 | 3249 |
Table 3 is the application of carboxylic polystyrene microsphere in a1-MG mensuration test kit of embodiment 1 preparation, according to the measurement result of table 3 and shown in Figure 2, experimental result shows, the a1-MG that the reagent that adopts embodiment 1 to prepare is researched and developed far above the CB096D microballoon that uses polymicrospheres the absorbancy changing value of each calibration object concentration determination measures test kit, when being 14 mg/L as calibration object concentration, the absorbancy changing value that the a1-MG of the CB096D microballoon research and development of polymicrospheres measures test kit is 602 units, and adopt the corresponding absorbancy changing value of reagent of embodiment 1 preparation that 1004 units are arranged fully, response intensity has surpassed 40% than the a1-MG mensuration test kit of the CB096D microballoon research and development of polymicrospheres, can see among Fig. 2 that the absorbancy of response curve on each calibration object concentration of the reagent of embodiment 1 preparation all is higher than the a1-MG mensuration test kit of the CB096D microballoon research and development of polymicrospheres, therefore we have drawn as drawing a conclusion: use the a1-MG of the CB096D microballoon research and development of polymicrospheres to measure test kit, response intensity is low, simultaneously can not solve the problem of microballoon aggegation, microballoon aggegation rate surpasses 20%, and stability has only tens days.Use embodiment 1, we can see the test kit response intensity made considerably beyond the CB096D microballoon of polymicrospheres, and the test kit cost directly descends 30%, and the while has solved the problem of microballoon aggegation fully, and is stable more than 1 year.
Table 4
| Retinol conjugated protein calibration object concentration (mg/L) | Embodiment 1 | The CB091E microballoon of polymicrospheres |
| 0 | -25 | -7 |
| 11 | 1302 | 750 |
| 22 | 2856 | 1680 |
| 45 | 5900 | 3507 |
| 90 | 13200 | 8215 |
Table 4 is the application of carboxylic polystyrene microsphere in retinol conjugated protein mensuration test kit of embodiment 1 preparation, adopt the reagent of embodiment 1 preparation that the absorbancy changing value of each calibration object concentration determination is measured test kit far above the retinol conjugated protein of the CB091E microballoon research and development of using polymicrospheres, when being 11 mg/L as calibration object concentration, the absorbancy changing value that the retinol conjugated protein of the CB091E microballoon research and development of polymicrospheres is measured test kit is 750 units, and adopt the corresponding absorbancy changing value of reagent of embodiment 1 preparation that 1302 units are arranged fully, response intensity is measured test kit than the retinol conjugated protein of the CB091E microballoon research and development of polymicrospheres and has been surpassed 70%, can see among Fig. 3 that the absorbancy of response curve on each calibration object concentration of the reagent of embodiment 1 preparation all is higher than the retinol conjugated protein mensuration test kit of the CB091E microballoon research and development of polymicrospheres, referring to shown in Figure 3, experiment shows, use the retinol conjugated protein of the microballoon research and development of embodiment 1 to measure test kit, the CB091E microballoon of the far super polymicrospheres of response intensity.Behind the microballoon of Application Example 1, when certain auxiliary material add-on is 5 times of CB091E microballoon of polymicrospheres, reagent still can be avoided the microballoon aggegation, and the anti-freezing effect that reagent is described is its 5 times at least, and the microballoon of use embodiment 1 is with 25% of direct saving cost.Simultaneously, exactly because the superpower response intensity of the test kit that this microballoon is researched and developed, it is the test kit that a present domestic unique family can measure urine and blood preparation simultaneously that the retinol conjugated protein of our research and development is measured test kit.
Table 5
| Bladder chalone C calibration object concentration (mg/L) | Embodiment 2 | The CB0104D microballoon of polymicrospheres |
| 0 | -17.5 | -8.75 |
| 0.5 | 327.5 | 164 |
| 1 | 766.5 | 383.75 |
| 2 | 1723 | 862.5 |
| 4 | 3552 | 1778 |
| 8 | 6756.5 | 3382.25 |
Table 5 is that the polystyrene microsphere of example 2 preparations is in the application of bladder chalone C determining reagent kit, the bladder chalone C determining reagent kit that the reagent that adopts embodiment 2 to prepare is researched and developed far above the CB0104D microballoon that uses polymicrospheres the absorbancy changing value of each calibration object concentration determination, when being 0.5 mg/L as calibration object concentration, the absorbancy changing value of the bladder chalone C determining reagent kit of the CB0104D microballoon research and development of polymicrospheres is 164 units, and adopt the corresponding absorbancy changing value of reagent of embodiment 2 preparations that 327.5 units are arranged fully, response intensity is 2 times of bladder chalone C determining reagent kit of the CB0104D microballoon research and development of polymicrospheres, can see among Fig. 5 that the absorbancy of response curve on each calibration object concentration of reagent of embodiment 2 preparation is all far above the bladder chalone C determining reagent kit of the CB0104D microballoon research and development of polymicrospheres, the response intensity height, low side response intensity height particularly, the mensuration that is conducive to urine specimen, experiment shows, use the bladder chalone C determining reagent kit of the microballoon research and development of embodiment 2, response intensity is far above the CB0104D microballoon of polymicrospheres, embodiment 2 microballoons can reach to concentrate and produce (the reagent concentrated solution of making 1 L can be diluted to 2-3 L) in addition, (concentration is too high and the CB0104D microballoon of polymicrospheres can not concentrate production, its microballoon can serious aggegation), so the production efficiency of embodiment 2 microballoons is far above its (be its 2-3 doubly); In addition, about 60% the raw material that embodiment 2 microballoons only need add the CB0104D microballoon of polymicrospheres just can reach identical response intensity with the reagent of the CB0104D microballoon research and development of polymicrospheres, and cost directly descends 40%.
Table 6
| B2-MG calibration object concentration (mg/L) | Embodiment 2 | The CB0130E microballoon of polymicrospheres |
| 0 | -13 | -19 |
| 1.5 | 782 | 397 |
| 4.5 | 3634.5 | 1670 |
| 9 | 8219.5 | 3813.5 |
| 18 | 11976 | 6557 |
Table 6 is the polystyrene microsphere of example 2 preparations is measured test kit at B2-MG application; The B2-MG that the reagent that adopts embodiment 2 to prepare is researched and developed far above the CB0130E microballoon that uses polymicrospheres the absorbancy changing value of each calibration object concentration determination measures test kit, when being 1.5 mg/L as calibration object concentration, the absorbancy changing value that the B2-MG of the CB0130E microballoon research and development of polymicrospheres measures test kit is 397 units, and adopt the corresponding absorbancy changing value of reagent of embodiment 2 preparations that 782 units are arranged fully, response intensity is higher 1 times than the B2-MG mensuration test kit of the CB0130E microballoon research and development of polymicrospheres, can see among Fig. 5 that the absorbancy of response curve on each calibration object concentration of the reagent of embodiment 2 preparation all measure test kit far above the B2-MG of the CB0130E microballoon research and development of polymicrospheres, use the test kit of the microballoon research and development of example 2 simultaneously, directly descend more than 30% at the cost aspect the raw material.
Can see from embodiment 1 and embodiment 2, same a kind of microballoon can satisfy the requirement of 2 kinds of reagent simultaneously, and the performance of reagent will be got well much than the reagent that adopts the research and development of polymicrospheres microballoon, simultaneously because the microballoon price of new Cheng Ziyan only is 1% of polymicrospheres microballoon, this makes our cost of reagent generally descend more than 20% even has reached 40%.
Table 7
| Myohaemoglobin calibration object concentration (mg/L) | Embodiment 2 | The CB0267D microballoon of polymicrospheres |
| 0 | -89 | -23 |
| 110 | 439 | 135 |
| 220 | 1204.5 | 350 |
| 440 | 3316 | 760 |
| 880 | 6972 | 1920 |
Table 7 is the polystyrene microsphere of example 3 preparations is measured test kit at myohaemoglobin application, adopt the reagent of embodiment 3 microballoons preparation that the absorbancy changing value of each calibration object concentration determination is measured test kit far above the myohaemoglobin of the CB0267D microballoon research and development of using polymicrospheres, when being 110 ng/L as calibration object concentration, the absorbancy changing value that the myohaemoglobin of the CB0267D microballoon research and development of polymicrospheres is measured test kit is 135 units, and adopt the corresponding absorbancy changing value of reagent of embodiment 3 preparations that 439 units are arranged fully, it is high 3 times that response intensity is measured test kit than the myohaemoglobin of the CB0267D microballoon research and development of polymicrospheres, can see among Fig. 6 embodiment 3 preparation reagent the absorbancy of response curve on each calibration object concentration all considerably beyond the myohaemoglobin of CB0267D microballoon research and development of polymicrospheres measure test kit, as the reagent of this trace detection of picture myohaemoglobin, the size of response intensity is reagent performance quality and important evaluating index thereof.Experiment shows, uses the myohaemoglobin of the microballoon research and development of embodiment 3 to measure test kit, and response intensity is considerably beyond the CB0267D microballoon of polymicrospheres, reagent excellent property.
Claims (9)
1. preparation technology who is applied to strengthen than the polystyrene microsphere of turbid reagent, it is characterized in that, reaction system comprises outer water, polymerization single polymerization monomer and function monomer, and the component of described outer water and content are: sodium lauryl sulphate 0.1-2g, polyethylene glycol 6000 2-16g, sodium-chlor 0.1-3g, purified water 400-600mL; The component of polymerization single polymerization monomer and content are: vinylbenzene 50-100mL, Vinylstyrene 0.5-1.0 mL; The component of function monomer and content are: ethyl propenoate 2-16mL, boric acid borate buffer solution 10-60mL; This preparation technology comprises the steps:
(1) configuration of outer water: accurately measure purified water according to the content ratio of outer water and place dissolution vessel, accurately take by weighing sodium lauryl sulphate, polyethylene glycol 6000 and sodium-chlor again in dissolution vessel, stirring and dissolving;
(2) purifying of polymerization single polymerization monomer: by measuring vinylbenzene and Vinylstyrene containing of polymerization single polymerization monomer in separating funnel, add sodium hydroxide solution and shake up, the stopper in the desolventizing is drawn unnecessary sodium hydroxide with purified water then;
(3) preparation of emulsion: stir the outer water for preparing and simultaneously the polymerization single polymerization monomer behind the purifying slowly is added dropwise to the outer aqueous phase for preparing, drip the mixing back and with ultrasonic instrument is ultrasonic it is uniformly dispersed;
(4) polyreaction: finely dispersed emulsion is poured in the reaction vessel, stirring heating, after treating that temperature rises to 65-85 ℃, add the initiator initiation reaction, after reaction 30-60min generates the polystyrene microsphere of no function group, add function monomer, reacted 5.5-7.5 hour, obtain carboxylic polystyrene microsphere.
2. a kind of preparation technology who is applied to strengthen than the polystyrene microsphere of turbid reagent according to claim 1 is characterized in that, the rotating speed that stirs in the described step (1) is 500-800rpm.
3. a kind of preparation technology who is applied to strengthen than the polystyrene microsphere of turbid reagent according to claim 1 is characterized in that, the quality percentage composition of sodium hydroxide solution is 5% in the described step (2).
4. a kind of preparation technology who is applied to strengthen than the polystyrene microsphere of turbid reagent according to claim 1 is characterized in that, the rotating speed that stirs in the described step (3) is 600rpm.
5. a kind of preparation technology who is applied to strengthen than the polystyrene microsphere of turbid reagent according to claim 1 is characterized in that, the power 40kHz of ultrasonic instrument in the described step (3), and it is ultrasonic that to make the time of its dispersion be 10-30min.
6. a kind of preparation technology who is applied to strengthen than the polystyrene microsphere of turbid reagent according to claim 1 is characterized in that the initiator in the described step (4) is ammonium persulphate.
7. a kind of preparation technology who is applied to strengthen than the polystyrene microsphere of turbid reagent according to claim 1 is characterized in that, function monomer divides 2 to 4 addings in the described step (4), and the amount that at every turn adds function monomer equates.
8. a kind of preparation technology who is applied to strengthen than the polystyrene microsphere of turbid reagent according to claim 7 is characterized in that, function monomer divides 4 addings in the described step (4).
9. according to claim 1 or 8 described a kind of preparation technologies that are applied to strengthen than the polystyrene microsphere of turbid reagent, it is characterized in that described function monomer is that ethyl propenoate is scattered in the solution that the boric acid borate buffer solution constitutes.
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| CN106674403A (en) * | 2017-01-03 | 2017-05-17 | 宏葵生物（中国）有限公司 | Preparation method of polystyrene microspheres for enhancing immunoturbidimetry and application thereof |
| CN108676112A (en) * | 2018-05-25 | 2018-10-19 | 苏州泽漫生物技术有限公司 | The preparation method of monodisperse solvent resistant high-carboxyl-content polystyrene microsphere |
| CN111892736B (en) * | 2020-08-13 | 2022-08-26 | 上海科华生物工程股份有限公司 | Polystyrene microsphere for improving sensitivity of latex turbidimetry and preparation method thereof |
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