CN104001486B - A kind of preparation method of hydrophily Sulfa drugs molecule trace solid-phase extraction column - Google Patents
A kind of preparation method of hydrophily Sulfa drugs molecule trace solid-phase extraction column Download PDFInfo
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Abstract
The invention belongs to technical field of chemical detection, be specifically related to a kind of preparation method of hydrophily Sulfa drugs molecule trace solid-phase extraction column.The preparation method of this hydrophily Sulfonamides molecularly imprinted solid phase extraction column, comprises the steps: that (1) is by mass polymerization synthesis hydrophilic sulfamido molecularly imprinted polymer; (2) imprinted polymer of step (1) gained is characterized, determine the existence of trace binding site; (3) polypropylene solid-phase extraction column is filled in.Prepared hydrophily solid-phase extraction column has powerful adsorption function, stronger specificity, preparation cost that the rate of recovery is high and lower, improves the shortcoming that the required quantity of solvent of traditional Sample Pretreatment Technique is large simultaneously.Can be directly used in the detection of ten kinds of Sulfonamides in animal derived food, it has the feature of high-selectivity adsorption and efficiently concentrating to sulfa drugs, and this solid-phase extraction column may be used for the detection of Sulfonamides in complete aqueous phase.
Description
Technical field
The invention belongs to technical field of chemical detection, be specifically related to a kind of preparation method of hydrophily Sulfa drugs molecule trace solid-phase extraction column, especially its in animal derived food to the enrichment of sulfamethyldiazine, sulfamethazine, sulphathiazole, sulfamethyldiazine, sulfadoxine, cistosulfa, 5-methoxysulfadiazine, sinomin, kynix and NU-445 10 kinds of sulfa drugs be separated.
Background technology
Sulfonamides is one of maximum antimicrobial of current use amount; be widely used for protection with its wide spectrum, the feature that efficient, consumption is few and control biological disease; but having research to point out at present, that excessive use Sulfonamides can cause it in edible tissue is residual; and then harm is produced to the health of human body; such as, allergic reaction, the harm suppressing Leukocytopoiesis and urinary system etc.So increasing scholar produces the concern of height to its residue detection in food.In order to ensure the security of food and the healthy of the mankind, many countries have customized the maximum limitation of Sulfonamides in food and have remained in the world, and wherein European Union and China specify that the total amount of Sulfonamides in food can not more than 100 μ g/L.
Residual in food of Sulfonamides is trace, simultaneously due to the complexity of food substrate, when detecting Sulfonamides, needs more complicated pretreatment process, brings certain difficulty to the detection of sample.Detecting the maximum pre-treating method of application to Sulfonamides is at present SPE.But current solid-phase extraction column exist poor specificity, a large amount of with an organic solvent, the shortcoming such as complex steps, bioaccumulation efficiency difference.Molecular imprinting is one of the method according to the principle preparation of bionic antibody with high selectivity, high adsorption molecular material.For Sulfonamides molecular imprinting, current preparation method is prepared in organic phase, and the adsorptivity in aqueous phase is poor.And the molecularly imprinted polymer prepared by current method can only be confined to have Specific adsorption to a certain Sulfonamides.So, study and a kind ofly may be used for multiple Sulfonamides enrichment in complete aqueous phase, with the molecularly imprinted solid phase extraction column be separated, there is comparatively profound significance.
At present about the invention of Sulfa drugs molecule trace solid-phase extraction column has two, one is the method (application publication number: CN102344527A) utilizing molecularly imprinted polymer purifying sulpha drugs, and another is preparation method and the application (application publication number: CN103289005A) of sulphonamide molecular-imprintingsolid-phase solid-phase extraction columella.In these two inventions, prepared Sulfa drugs molecule imprinted polymer, can only detect 3 kinds of sulfa drugs, and can not completely for the detection of aqueous sample.
Summary of the invention
The object of the invention is to the shortcoming overcoming traditional solid phase extraction techniques, is the preparation method that there are provided a kind of hydrophily Sulfa drugs molecule trace solid-phase extraction column.Hydrophily solid-phase extraction column prepared by the method has powerful adsorption function, stronger specificity, preparation cost that the rate of recovery is high and lower, improves the shortcoming that the required quantity of solvent of traditional Sample Pretreatment Technique is large simultaneously.
Another object of the present invention there are provided a kind of hydrophily Sulfa drugs molecule trace solid-phase extraction column in animal derived food to sulfamethazine, sulphadiazine, sulfamethyldiazine, the application that other sulfa drugs such as sulphathiazole detect, experiment proves, this solid-phase extraction column can be directly used in sulfamethazine in animal derived food, sulphadiazine, sulfamethyldiazine, sulphathiazole, sulfadoxine, 5-methoxysulfadiazine, sinomin, kynix NU-445 and cistosulfa ten kinds of sulfa drugs, it has the feature of high-selectivity adsorption and efficiently concentrating to sulfa drugs, and, this solid-phase extraction column may be used for the detection of Sulfonamides in complete aqueous phase.
The present invention is realized by following scheme:
A preparation method for hydrophily Sulfa drugs molecule trace solid-phase extraction column, comprises the steps:
(1) first by template molecule, function monomer and crosslinking agent, mix according to the ratio of mol ratio 0.1:4:6, by mass polymerization synthesis hydrophilic sulfamido molecularly imprinted polymer;
(2) imprinted polymer of step (1) gained is characterized, determine the existence of trace binding site;
(3) take Sulfa drugs molecule imprinted polymer particulate 0.050-0.200g, be filled in the polypropylene solid-phase extraction column of 5mL, load onto polyethylene sieve plate respectively at the two ends of filler, sieve plate is covered tightly, to obtain final product.
In the preparation method of above-mentioned hydrophily Sulfa drugs molecule trace solid-phase extraction column, described template molecule is sulfamethazine and sulphathiazole, and both molar ratios are 1:1.
In the preparation method of above-mentioned hydrophily Sulfa drugs molecule trace solid-phase extraction column, described function monomer is methacrylic acid (MAA) and hydrophily function monomer hydroxyethyl methacrylate (HEMA), and both molar ratios are 1:1; Described crosslinking agent is ethylene glycol dimethacrylate and 3-(trimethoxysilyl) one in propyl acrylate or two kinds.。
In the preparation method of above-mentioned hydrophily Sulfa drugs molecule trace solid-phase extraction column, described characterizing method comprises Dynamic Adsorption, Static Adsorption and specific adsorption.
The main implementation step of the experiment of above-mentioned Staticadsorption experiment, Dynamic Adsorption and specific adsorption is as follows:
1) Staticadsorption experiment: using the aqueous solution of the sulfamethazine of 30mg/L as adsorption liquid, accurately take the molecularly imprinted polymer 5 parts of 25mg, add the adsorption liquid of 5mL, vibrate 5min, 10min, 30min, 120min, 240min respectively.Centrifugation, gets supernatant, measures the concentration of sulfamethazine in supernatant under 268nm condition on ultraviolet-visible spectrophotometer.
2) Dynamic Adsorption experiment: accurately take the volumetric flask that 25mg hydrophily sulfonamide molecularly imprinted polymer is placed in 25mL, add the sulfamethazine aqueous solution of 5mL variable concentrations respectively, after shaking table vibration 30min, centrifugation, tests the concentration of sulfamethazine in supernatant under 268nm condition.And simultaneously parallelly do non-imprinted polymer and do control experiment.With adsorbance to the mapping of template molecule concentration, draw adsorption isothermal curve.
3) specific adsorption experiment: select the MTMC similar to template molecule structure, chlorine sulphur is grand, estriol is as the competitor of sulfa drugs, accurately take the imprinted polymer of 25.00mg and non-imprinted polymer, be placed in the volumetric flask of 25mL, respectively add the sulphathiazole of 10mg/L, sulphadiazine, sulfamethazine, sulfamethyldiazine, NU-445, kynix, 5-methoxysulfadiazine, MTMC, the mixed aqueous solution 5mL of the grand and estriol of chlorine sulphur, the centrifugal 15min of 3000rpm after vibration 30min, HPLC-DAD detector records each analyte concentration in supernatant, recording wavelength sulfa drugs is 270nm, MTMC is 210nm, estriol and chlorine sulphur grand be 230nm.According to comparing of supernatant and concentration of standard solution before and after absorption, calculate the adsorbance of often kind of material, distribution coefficient (Kd), selectivity factor (K) and relative selectivity coefficient (K).
In the preparation method of above-mentioned hydrophily Sulfonamides molecularly imprinted solid phase extraction column, the preparation process of described hydrophily Sulfa drugs molecule imprinted polymer is as follows:
(1) using the sulfamethazine of 0.05mmol and the sulphathiazole of 0.05mmol as template, be dissolved in pore-foaming agent, by mixed solution ultrasonic degas, make it mix;
(2) the function monomer methacrylic acid of 2mmol is joined in the Homogeneous phase mixing liquid prepared by step (1), vibrate on the oscillator, obtain prepolymerization system;
(3) in step 2) add hydrophily function monomer hydroxyethyl methacrylate (HEMA), vibration 1h in the prepolymerization system that obtains; Then crosslinking agent is added, vibration 1h; Finally add initator, vibration 0.5h, passes into nitrogen deoxygenation 5min, and at the atmosphere lower seal of nitrogen;
(4) at 60 DEG C of Water Under bath 24h, heat causes the polymerization system described in step (3), obtains the block molecularly imprinted polymer of hydrophily sulfonamide;
(5) the block molecularly imprinted polymer of gained in step (4) is sieved after grinding, sub-sieve obtains the particle diameter between 30-60 μm, underproof particle is removed, wrap up with qualitative filter paper, then in apparatus,Soxhlet's, 50h-110h is extracted with the extractant of 250mL, then use hydrochloric acid and the methanol wash 5h of 1mmol, dry to constant weight, obtain imprinted polymer particle for 75 DEG C.
In the preparation method of above-mentioned hydrophily Sulfa drugs molecule trace solid-phase extraction column, described pore-foaming agent is acetonitrile, and its consumption is 6mL.
In the preparation method of above-mentioned hydrophily Sulfa drugs molecule trace solid-phase extraction column, the speed of described vibration is 160 turns/min, and duration of oscillation is 3h.
In the preparation method of above-mentioned hydrophily Sulfa drugs molecule trace solid-phase extraction column, described hydrophily function monomer is hydroxyethyl methacrylate (HEMA), and its consumption is 2mmol.
In the preparation method of above-mentioned hydrophily Sulfa drugs molecule trace solid-phase extraction column, described crosslinking agent is the ethyleneglycol dimethacrylate (EDMA) of 3mmol and the 3-(trimethoxysilyl of 3mmol) propyl acrylate (γ-MAPS), described initator is azodiisobutyronitrile (AIBN), and consumption is 25mg.
In the preparation method of above-mentioned hydrophily Sulfa drugs molecule trace solid-phase extraction column, methyl alcohol and the formic acid mixed solution of described extractant to be volume ratio be 9:1.
In use, the using method of hydrophily Sulfa drugs molecule trace solid-phase extraction column of the present invention is as follows:
1) by after SPE column filling, activate with the methyl alcohol of 3mL and the water of 3mL and balance solid-phase extraction column;
2) under the condition vacuumized, sample 50mL is added;
3) with the distilled water drip washing solid-phase extraction column of 3mL, removing is not by the object that adsorbs and other impurity;
4) by the methanol-eluted fractions 1 time of 3mL, eluent is collected, to be detected.
Beneficial effect of the present invention is:
(1) the hydrophily Sulfa drugs molecule trace solid-phase extraction column prepared by the present invention all has specific adsorption function to sulfa drugs in sulphathiazole, sulfamethazine, sulfamethyldiazine, sulphadiazine, sulfadoxine, cistosulfa, 5-methoxysulfadiazine, kynix, sulfamoxole and NU-445 10, may be used for this ten kinds of Sulfonamides retention analysis in animal derived food.
(2) hydrophily Sulfa drugs molecule trace solid-phase extraction column of the present invention may be used for the retention analysis of sulfa drugs in the sample of complete water sample, the non-hydrophilic material of conventional method synthesis carries out all in organic solvent in whole testing process, used solvent can up to milliliter up to a hundred, and the hydrophilic material prepared by this method does not need to use organic solvent in testing process, all can carry out in aqueous, solve the difficult problem that in traditional detection method, organic solvent use amount is large.
(3) the more commercial solid-phase extraction column of hydrophily Sulfa drugs molecule trace solid-phase extraction column of the present invention, such as C18, neutral alumina, OasisHLB solid-phase extraction column is compared, the cost of its synthesis is lower, and can recycled for multiple times, solve the high price of commercialization solid-phase extraction column and a disposable difficult problem.
Accompanying drawing explanation
The curve of adsorption kinetics of the aqueous solution on 25mg molecular engram material of the sulfamethazine of Fig. 1: 5mL30mg/L
Fig. 2: imprinted polymer and non-imprinted polymer are to the adsorption isothermal curve of sulfamethazine
Fig. 3: the Scatchard of imprinted polymer and non-imprinted polymer analyzes.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described, so that those skilled in the art more understands the present invention, but does not therefore limit the present invention.
Embodiment 1
(1) preparation of hydrophily sulfanilamide (SN) molecularly imprinted polymer
First the sulfamethazine of 0.05mmol and the sulphathiazole of 0.05mmol are dissolved in the acetonitrile of 6mL, after ultrasonic 15min, add the function monomer methacrylic acid of 2mmol.On the oscillator with the speed oscillation 3h of 160 turns/min, form pre-polymer solution.Subsequently, add 2mmol hydrophily function monomer hydroxyethyl methacrylate (HEMA) in above-mentioned pre-polymer solution system after, vibration 1h; Then crosslinking agent (ethyleneglycol dimethacrylate of 3mmol and the 3-(trimethoxysilyl of the 3mmol) propyl acrylate of 6mmol is added), vibration 1h; Finally add the initator azodiisobutyronitrile (AIBN) of 25mg, vibration 0.5h.Pass into nitrogen deoxygenation 5min, and at the atmosphere lower seal of nitrogen; By thermal-initiated polymerization under water-bath 60 DEG C of conditions, water bath time is 24h.Bulk polymer is obtained after reaction terminates.Wrap up after polymer abrasive with qualitative filter paper, then extracting 80h(extractant with apparatus,Soxhlet's is methyl alcohol: formic acid is 9:1), until detect without template molecule.Then use the hydrochloric acid of 20mL1mmol and the methanol wash 5h of 20mL, dry to constant weight, obtain imprinted polymer particle for 75 DEG C.The preparation of non-imprinted polymer is not except adding except template molecule, and other step is identical with above-mentioned steps.
(2) sign of hydrophilic molecular engram polymer
2.1 using the aqueous solution of the sulfamethazine of 30mg/L as adsorption liquid, accurately take the molecularly imprinted polymer 5 parts of 25mg, add the adsorption liquid of 5mL, vibrate 5min, 10min, 30min, 120min, 240min respectively.Centrifugation, gets supernatant, measures the concentration of sulfamethazine in supernatant under 270nm condition on ultraviolet-visible spectrophotometer.As shown in Figure 1, the imprinted polymer of this method synthesis has the good rate of adsorption and mass transfer rate to sulfamethazine.When adsorption time is 5min, adsorbance is 51.25% of saturated extent of adsorption; When adsorption time is 30min, adsorbance can reach capacity 91.19% of adsorbance, substantially reaches adsorption equilibrium.And the time that the polymer of conventional method synthesis reaches adsorption equilibrium needs several hours, the method substantially reduces adsorption time, significantly improves the mass transfer rate of material.
In order to determine the rate-limiting step of polymer in adsorption process, the simulation of primary adsorption dynamics, secondary absorption dynamics, Particle diffusion equation and Elovich equation curve is carried out to the data of experiment gained.Data are brought in each equation, passes through R
2size judge whether whether analog result conform to theoretical model.Analog result is in table 1.Its curve of adsorption kinetics is shown in Fig. 1.
As shown in Table 1, compared with other model, the linear dependence of secondary absorption kinetic simulation pseudocurve is best, can reach R
2be 0.9985, present pole significant correlation level.Accurate secondary absorption kinetic model is thought, two reactions can occur in adsorption process: one is the reaction reaching balance fast, and two is the long response times controlling the whole reaction time, and these two reactions may be carried out successively, also may carry out simultaneously.
2.2 accurately take the volumetric flask that 25mg hydrophily sulfonamide molecularly imprinted polymer is placed in 25mL, add the sulfamethazine aqueous solution of 5mL variable concentrations respectively, after shaking table vibration 30min, centrifugation, tests the concentration of sulfamethazine in supernatant under 270nm condition.And simultaneously parallelly do non-imprinted polymer and do control experiment.With adsorbance to the mapping of template molecule concentration, draw adsorption isothermal curve.Adsorption equilibrium curve as shown in Figure 2, as seen from Figure 2, when the concentration of adsorption liquid is when very low concentration range, the adsorbance difference of imprinted polymer and non-imprinted polymer is less, but along with the increase of adsorption liquid concentration, both adsorbances all have increase in various degree, and its difference is also more and more obvious.When the concentration of the sulfamethazine aqueous solution is 30mg/L, the adsorbance of imprinted polymer is 0.658mg/g, the adsorbance of non-imprinted polymer is 0.232mg/g, and the adsorbance of imprinted polymer is approximately 2.83 times of non-imprinted polymer adsorbance, illustrates that the imprinting effect of this material is better.
2.3Scatchard analyze
The Scatchard obtained data being used for imprinted polymer and non-imprinted polymer analyzes.Analysis result is shown in Fig. 3.
Scatchard equation: Q/C=Q/b+Qmax/b
In equation, C refers to the initial concentration of solution, and Q refers to adsorption capacity when reaching adsorption equilibrium, and Qmax refers to maximum saturation adsorption capacity, to map and obtain Scatchard equation with Q/C to Q.Qmax and Kd of polymer can be obtained by Scatchard slope of a curve and intercept.
As seen from the figure, the Scatchard of imprinted polymer is a linear good curve, and regression equation is y=-0.0024x+0.0273, and coefficient correlation is 0.9924.Wherein, Qmax is 11.37mg/g, Kd is 4.17mg/mL.Illustrate that the imprinted polymer that the method is synthesized has certain binding site, to template molecule, there is specific absorption affinity.But not imprinted polymer is due to the scrambling in conjunction with strength, so can not get linear equation.
2.4 competitive Adsorption experiments
Select the MTMC similar to template molecule structure, chlorine sulphur is grand, estriol is as the competitor of sulfa drugs, accurately take the imprinted polymer of 25.00mg and non-imprinted polymer, be placed in the volumetric flask of 25mL, respectively add the sulphathiazole of 10mg/L, sulphadiazine, sulfamethazine, sulfamethyldiazine, NU-445, kynix, 5-methoxysulfadiazine, MTMC, the mixed aqueous solution 5mL of the grand and estriol of chlorine sulphur, the centrifugal 15min of 3000rpm after vibration 30min, HPLC-DAD detector records each analyte concentration in supernatant, recording wavelength sulfa drugs is 270nm, MTMC is 210nm, estriol and chlorine sulphur grand be 230nm.According to comparing of supernatant and concentration of standard solution before and after absorption, calculate the adsorbance of often kind of material, distribution coefficient (K
d), selectivity factor (K) and relative selectivity coefficient (K
,).The results are shown in Table 2.
As can be seen from Table 2, imprinted polymer will be far longer than the adsorption capacity of non-imprinted polymer to sulfa drugs to the adsorbance of sulfa drugs.And imprinted polymer is less to MTMC, chlorine sulphur adsorbance that is grand and estriol, be starkly lower than the adsorbance of non-imprinted polymer and estriol grand to MTMC, chlorine sulphur.Illustrate that the sorbing material synthesized by this method has stronger selective recognition to 10 kinds of sulfa drugs.
(3) preparation of solid-phase extraction column
Take Sulfa drugs molecule imprinted polymer particulate 0.050-0.200g, be filled in the polypropylene solid-phase extraction column of 5mL, load onto polyethylene sieve plate respectively at the two ends of filler, sieve plate is covered tightly, to obtain final product.
The application of hydrophily sulfa drugs solid-phase extraction column prepared by embodiment 2
(1) extraction of ten kinds of sulfa drugs in pork
Bought pork sample is placed in mixer homogeneous to be placed on-20 DEG C of refrigerators and to preserve.Accurately take 1.00g pork sample and be placed in 100mL beaker, analyze thing mixed solution for ten kinds of mark-on variable concentrations.Protein denaturation is made, except deproteinize is to the interference analyzing quality testing survey with the ultrasonic 15min of 3mL methyl alcohol.In triplicate.Collect supernatant centrifugal 15min under 3000r/min rotating speed.Get supernatant through 0.22 μm of membrane filtration, proceed in 50mL volumetric flask, after being settled to scale, treat Solid phase extraction.
(2) purify
Before loading, first activate successively by 3mL methyl alcohol and 3mL deionized water and balance solid-phase extraction column, using the 50mL10 kind sulfonamide hybrid standard aqueous solution as sample liquid, loading enrichment purifies.Target analytes is attracted on MISPE post, is not flowed out with waste liquid by the part of adsorbing.MISPE post with 1.00mL/min flow velocity wash-out MISPE solid-phase extraction column, collects eluent with 2.00mL methanol solution, at room temperature dries up the methanol solution redissolution of rear 1.0mL with nitrogen stream, after 0.45 μm of membrane filtration, gets 20 μ L direct injected HPLC and detect.After enrichment purification, the methyl alcohol of MISPE post 5mL and 5mL distilled water are thoroughly washed, uses in order to next preenrichment.
(3) rate of recovery of high effective liquid chromatography for measuring 10 kinds of sulfonamides
Chromatographic condition: chromatographic column ThermoC18 post (5um, 4.6mm × 250mm) mobile phase A: the aqueous solution of methanol as mobile phase B:0.1%, the ratio of mobile phase A and Mobile phase B is 25:75.Determined wavelength is 270nm.
After measured, the recovery of standard addition of 10 kinds of sulfa drugs in pork, at 73.9%-85.4%, the results are shown in Table 3.
Claims (8)
1. a preparation method for hydrophily Sulfa drugs molecule trace solid-phase extraction column, comprises the steps:
(1) first by template molecule, function monomer and crosslinking agent, mix according to the ratio of mol ratio 0.1:4:6, by mass polymerization synthesis hydrophilic sulfamido molecularly imprinted polymer; Described template molecule is sulfamethazine and sulphathiazole, and both molar ratios are 1:1;
Described function monomer is methacrylic acid and hydrophily function monomer hydroxyethyl methacrylate, and both molar ratios are 1:1; Described crosslinking agent is ethylene glycol dimethacrylate and 3-(trimethoxysilyl) one in propyl acrylate or two kinds;
(2) imprinted polymer of step (1) gained is characterized, determine the existence of trace binding site;
(3) take Sulfa drugs molecule imprinted polymer particulate 0.050-0.200g, be filled in the polypropylene solid-phase extraction column of 5mL, load onto polyethylene sieve plate respectively at the two ends of filler, sieve plate is covered tightly, to obtain final product.
2. the preparation method of a kind of hydrophily Sulfa drugs molecule trace solid-phase extraction column according to claim 1, it is characterized in that, described characterizing method comprises Dynamic Adsorption, Static Adsorption and specific adsorption.
3. the preparation method of a kind of hydrophily Sulfa drugs molecule trace solid-phase extraction column according to claim 1, it is characterized in that, the preparation process of described hydrophily Sulfa drugs molecule imprinted polymer is as follows:
(1) using the sulfamethazine of 0.05mmol and the sulphathiazole of 0.05mmol as template, be dissolved in pore-foaming agent, by mixed solution ultrasonic degas, make it mix;
(2) the function monomer methacrylic acid of 2mmol is joined in the Homogeneous phase mixing liquid prepared by step (1), vibrate on the oscillator, obtain prepolymerization system;
(3) in step 2) add hydrophily function monomer hydroxyethyl methacrylate, vibration 1h in the prepolymerization system that obtains; Then crosslinking agent is added, vibration 1h; Finally add initator, vibration 0.5h, passes into nitrogen deoxygenation 5min, and at the atmosphere lower seal of nitrogen;
(4) at 60 DEG C of Water Under bath 24h, heat causes the polymerization system that step (3) obtains, and obtains the block molecularly imprinted polymer of hydrophily sulfonamide;
(5) the block molecularly imprinted polymer of gained in step (4) is sieved after grinding, sub-sieve obtains the particle diameter between 30-60 μm, underproof particle is removed, wrap up with qualitative filter paper, then in apparatus,Soxhlet's, 50h-110h is extracted with the extractant of 250mL, then use hydrochloric acid and the methanol wash 5h of 1mmol, dry to constant weight, obtain hydrophily Sulfa drugs molecule imprinted polymer for 75 DEG C.
4. the preparation method of a kind of hydrophily Sulfa drugs molecule trace solid-phase extraction column according to claim 3, it is characterized in that, described pore-foaming agent is acetonitrile, and its consumption is 6mL.
5. the preparation method of a kind of hydrophily Sulfa drugs molecule trace solid-phase extraction column according to claim 3, it is characterized in that, the speed of described vibration is 160 turns/min, and duration of oscillation is 3h.
6. the preparation method of a kind of hydrophily Sulfa drugs molecule trace solid-phase extraction column according to claim 3, it is characterized in that, described hydrophily function monomer is hydroxyethyl methacrylate, and its consumption is 2mmol.
7. the preparation method of a kind of hydrophily Sulfa drugs molecule trace solid-phase extraction column according to claim 3, it is characterized in that, described crosslinking agent is the ethyleneglycol dimethacrylate of 3mmol and the 3-(trimethoxysilyl of 3mmol) propyl acrylate, described initator is azodiisobutyronitrile, and consumption is 25mg.
8. the preparation method of a kind of hydrophily Sulfa drugs molecule trace solid-phase extraction column according to claim 3, is characterized in that, methyl alcohol and the formic acid mixed solution of described extractant to be volume ratio be 9:1.
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| CN106810638A (en) * | 2016-12-23 | 2017-06-09 | 齐鲁工业大学 | The preparation method and application of Sulfonamides hydrophilic magnetic molecular engram material |
| CN107233873B (en) * | 2017-07-24 | 2019-03-29 | 齐鲁工业大学 | There is the preparation method of the solid-phase micro-extraction fibre of specificity to sulfa drugs |
| CN109180864B (en) * | 2018-07-18 | 2021-05-18 | 江苏全给净化科技有限公司 | Molecularly imprinted polymer material for purifying sulfonamides in water and application thereof |
| EP3721985A1 (en) * | 2019-04-08 | 2020-10-14 | Tallinn University of Technology | Molecularly imprinted polymers sensors for sulfonamides |
| CN112090411B (en) * | 2020-08-06 | 2023-07-18 | 河南科技学院 | Magnetic material for analyzing sulfonamide antibiotics and detection method of sulfonamide antibiotics |
| CN113686832B (en) * | 2021-08-20 | 2022-08-23 | 江南大学 | Ultrasensitive recognition dot matrix array detection method for sulfonamide antibiotics |
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