An adsorption material for aminoglycoside antibiotics, and its preparation method and application
By preparing aminoglycoside adsorption materials with mesoporous structures and utilizing cross-linking and grafting reactions between functional monomers and magnetic templates, the problem of poor adsorption efficiency of aminoglycoside antibiotics in the existing technology is solved, and efficient adsorption and separation effects are achieved.
Patent Information
- Application Number
- CN202311311216.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-11
- Publication Date
- 2025-09-30
- Estimated Expiration
- 2043-10-11
AI Technical Summary
The adsorption efficiency of aminoglycoside antibiotics in the existing technology is poor, and separation is difficult.
An adsorption material with a mesoporous structure is prepared through the cross-linking reaction of 2,5-divinyl-1,4-benzenedicarboxaldehyde and 1,3,5-tris(4-aminophenyl)benzene, combined with the grafting reaction of the thiol group of 3-mercapto-2-butanone and the intermediate monomer. The functional monomers are then arranged in a direction using a magnetic template to form specific cavities or channels, thereby enhancing the recognition ability of aminoglycosides.
The surface area and adsorption selectivity of the adsorption material are improved, efficient adsorption and selective separation of aminoglycosides are achieved, and the material has good reusability.
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Figure CN117225381B_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of adsorption materials, and in particular relates to an adsorption material for aminoglycoside antibiotics, a preparation method thereof and an application thereof. Background Art
[0002] There are many types of antibiotics. Among them, aminoglycosides and macrolides are commonly used veterinary antibiotics in agricultural production and are also commonly used animal growth promoters. Therefore, residues of these two classes of antibiotics are common in animal-derived foods. Aminoglycoside antibiotics are highly polar, alkaline compounds that are not retained in reversed-phase chromatography. Their structures lack chromophores and, therefore, lack UV and / or fluorescent absorption. Therefore, aminoglycosides are very difficult to separate and detect.
[0003] Patent CN 116099513 A discloses a method for preparing a solid-phase extraction column filler specifically for aminoglycosides and its application. The method for preparing the filler comprises the following steps: adding a pre-configured dispersant aqueous solution and a mixture of a crosslinker, a porogen, and an initiator to a reactor, heating the mixture to 45-55°C for polymerization for 1-4 hours to form polymer microspheres; continuously adding a mixture of an initiator, a functional monomer, and a template molecule, heating the mixture to 70-85°C, and reacting to obtain product microspheres; and then removing some of the template molecules by etching. The resulting specific cavities have good selectivity for aminoglycosides, but the adsorption rate still needs to be improved. Summary of the Invention
[0004] The purpose of the present invention is to provide an adsorption material for aminoglycoside antibiotics, a preparation method and application thereof, so as to solve the technical problems of poor adsorption efficiency and complicated separation of adsorption materials in the prior art.
[0005] In order to achieve the above object, the present invention adopts the following technical solutions:
[0006] The present invention provides a method for preparing an adsorption material for aminoglycoside antibiotics, comprising the following steps:
[0007] Step (1) mixing a functional monomer, a cross-linking agent, 1-butanol, 1,2-dichlorobenzene and an acetic acid aqueous solution, subjecting the mixture to a freeze-thaw cycle, sealing, heating, filtering and washing to obtain an intermediate monomer;
[0008] The structural formula of the intermediate monomer is as follows:
[0009]
[0010] In the above process, the aldehyde group of the functional monomer 2,5-divinyl-1,4-benzenedicarboxaldehyde reacts with the amino group of the cross-linking agent 1,3,5-tris(4-aminophenyl)benzene to form a cross-linking polymerization, and the intermediate monomer has a mesoporous structure.
[0011] Step (2) Under N2 atmosphere, the intermediate monomer, magnetic template, 3-mercapto-2-butanone and benzenetrifluoromethane are mixed, stirred, filtered, washed, the template is eluted, and vacuum dried to obtain an adsorption material.
[0012] The structural formula of the adsorption material is as follows:
[0013]
[0014] In the above process, the double bond of the intermediate monomer is grafted with the thiol group of 3-mercapto-2-butanone through a thiol-olefin reaction, and the carbonyl group in 3-mercapto-2-butanone forms a hydrogen bond with the amino group in the template to directional arrange the functional monomers.
[0015] Preferably, the method for preparing the magnetic template comprises the following steps:
[0016] S1: 1-2 g of Fe3O4 nanoparticles were added to 500-1000 mL of anhydrous ethanol and ultrasonically treated for 15-20 min. 10-20 mL of ethyl silicate was then added dropwise and stirred for 1-3 h. The mixture was centrifuged at 9000-11000 r / min for 10-20 min. The centrifuged solid was washed 3-5 times with deionized water until the pH was neutral. The solid was dried with activated silica at 20-24 ° C for 12-36 h to obtain core-shell Fe3O4.
[0017] In the above process, silicon dioxide acts as a shell material wrapped around the surface of Fe3O4 to form a core-shell structure Fe3O4.
[0018] S2: 0.2-0.4 g core-shell Fe3O4, 40-80 mL deionized water, 160-320 mL ethanol and 1.5-3 mL 25 v / v% ammonia water were mixed, ultrasonically treated for 25-35 min, mechanically stirred at a speed of 150-250 r / min at 20-30 ° C for 25-30 min, then 0.5-1.1 g template molecule was added, and mechanically stirred at a speed of 150-250 r / min at 20-30 ° C for 50-70 min, and then 2-4 mL ethyl silicate was slowly added. The mixture was stirred at a speed of 150-250 r / min at 20-30 ° C for 60-120 min. After separation with an external magnet, it was washed alternately with 50-100 mL ethanol and 50-100 mL deionized water for 3-5 times to obtain a magnetic template.
[0019] In the above process, the amino groups in the template react with ethyl silicate and the hydroxyl groups in the core-shell Fe3O4 to cross-link and obtain a magnetic template.
[0020] Preferably, the template molecule comprises at least one of tocopherol succinate, kanamycin sulfate, amikacin sulfate, neomycin sulfate, streptomycin sulfate and gentamicin sulfate.
[0021] More preferably, the template molecule includes at least one of tocopherol succinate and gentamicin sulfate.
[0022] Preferably, in step (1), the usage ratio of the functional monomer, the cross-linking agent, 1-butanol, 1,2-dichlorobenzene, and the acetic acid aqueous solution is (44-88) g:(56-112) g:(1-2) L:(1-2) L:(0.2-0.4) L.
[0023] Preferably, in step (1), the functional monomer is 2,5-divinyl-1,4-benzenedicarboxaldehyde; the cross-linking agent is 1,3,5-tris(4-aminophenyl)benzene; the molar concentration of the acetic acid aqueous solution is 6 mol / L; the number of freeze-thaw cycles is 3-5 times; the sealing method is sealed under vacuum; the heating conditions are: the heating temperature is 80-120°C and the heating time is 5-7h; and the washing method is: washing with tetrahydrofuran 3-5 times.
[0024] Preferably, in step (2), the usage ratio of the intermediate monomer, the magnetic template, 3-mercapto-2-butanone, and benzyltrifluoromethane is (25-50) g: (0.6-1.3) g: (12-25.1) g: (1-2) mL.
[0025] Preferably, in the step (2), the stirring treatment conditions are: the stirring treatment temperature is 70-90° C., and the stirring treatment time is 5-7 h; the washing method is: the precipitate is washed 3-5 times with tetrahydrofuran; the template elution method is: the template is eluted from the precipitate with a methanol-acetic acid mixture with a volume ratio of 9:1; the vacuum drying conditions are: the vacuum drying temperature is 50-70° C., and the vacuum drying time is 1-3 h.
[0026] The aminoglycoside antibiotic adsorption material is prepared by adopting the preparation method of the aminoglycoside antibiotic adsorption material.
[0027] The present invention also provides an adsorption material for aminoglycoside antibiotics as an extraction adsorbent, which is applied to the separation and enrichment of aminoglycoside antibiotics in an aqueous phase system.
[0028] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:
[0029] 1. In the present invention, an adsorption material with a high specific surface area is prepared by reacting the aldehyde group of 2,5-divinyl-1,4-benzenedicarboxaldehyde with the amino group of 1,3,5-tris(4-aminophenyl)benzene, and then reacting the double bond with the thiol group of 3-mercapto-2-butanone for grafting. During the formation of the adsorption material, the functional monomers can be oriented by adding template molecules, thereby giving the adsorption material a higher surface area. Aminoglycoside is used as a template to form a specific structure and function in the polymer. After the polymerization reaction, the intermediate monomer formed has cavities or channels that match the aminoglycoside. These cavities or channels can specifically interact with the structure, size and functional groups of the target molecule, have strong recognition ability for aminoglycoside, and have high selectivity and good sensitivity for aminoglycoside adsorption.
[0030] 2. The present invention reacts the thiol functional group of 3-mercapto-2-butanone with the double bond in the intermediate monomer to generate a sulfur-carbon bond that is a polar group capable of specifically interacting with aminoglycoside antibiotics. This increases the bonding amount of the functional monomer on the solid matrix surface, resulting in an adsorption material with superior adsorption capacity. After adsorption treatment, there is no significant matrix effect. After 12 cycles of capturing and releasing aminoglycoside antibiotics, it was found that the adsorption capacity and selectivity of the adsorption material for aminoglycoside antibiotics did not change significantly, indicating that the adsorption material has good reusability. BRIEF DESCRIPTION OF THE DRAWINGS
[0031] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.
[0032] Figure 1 The present invention is a flow chart of the preparation process of the adsorption material of aminoglycoside antibiotics. DETAILED DESCRIPTION
[0033] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.
[0034] Example 1
[0035] This embodiment discloses a method for preparing a magnetic template, comprising the following steps:
[0036] S1: 1.5 g of Fe3O4 nanoparticles were added to 750 mL of anhydrous ethanol and ultrasonically treated for 18 min. 15 mL of ethyl silicate was then added dropwise and stirred for 2 h. The mixture was centrifuged at 10,000 rpm for 15 min. The centrifuged solid was washed four times with deionized water until the pH was neutral and dried with activated silica at 22 °C for 24 h to obtain core-shell Fe3O4.
[0037] S2: 0.3 g of core-shell Fe3O4, 60 mL of deionized water, 240 mL of ethanol and 2.3 mL of 25 v / v% ammonia water were mixed, ultrasonically treated for 30 min, mechanically stirred at 200 r / min at 25 ° C for 28 min, then 1 g of template molecule was added, and mechanically stirred at 200 r / min at 25 ° C for 60 min, and then 3 mL of ethyl silicate was slowly added, and stirring was continued at 200 r / min at 25 ° C for 90 min. After separation with an external magnet, it was washed alternately with 75 mL of ethanol and 75 mL of deionized water 4 times to obtain a magnetic template.
[0038] Example 2
[0039] See Figure 1 As shown, this embodiment discloses a method for preparing an adsorption material for aminoglycoside antibiotics, comprising the following steps:
[0040] Step (1) 66 g of 2,5-divinyl-1,4-benzenedicarboxaldehyde, 82 g of 1,3,5-tris(4-aminophenyl)benzene, 1.5 L of 1-butanol, 1.5 L of 1,2-dichlorobenzene and 0.3 L of a 6 mol / L aqueous acetic acid solution were mixed, subjected to freeze-thaw cycles 3-5 times, sealed under vacuum, heated at 90° C. for 6 h, filtered, and washed 4 times with tetrahydrofuran to obtain an intermediate monomer;
[0041] Step (2) Under a nitrogen atmosphere, 37.5 g of the intermediate monomer, 0.9 g of the magnetic tocopherol succinate prepared in Example 1, 18.1 g of 3-mercapto-2-butanone, and 1.5 mL of benzyltrifluoromethane were mixed and stirred at 80° C. for 6 h. The mixture was filtered, and the precipitate was washed four times with tetrahydrofuran. The template tocopherol succinate was then eluted from the precipitate with a methanol-acetic acid mixture with a volume ratio of 9:1. The mixture was vacuum dried at 60° C. for 2 h to obtain an adsorption material.
[0042] Example 3
[0043] See Figure 1 As shown, this embodiment discloses a method for preparing an adsorption material for aminoglycoside antibiotics, comprising the following steps:
[0044] Step (1) 44 g of 2,5-divinyl-1,4-benzenedicarboxaldehyde, 112 g of 1,3,5-tris(4-aminophenyl)benzene, 1 L of 1-butanol, 1 L of 1,2-dichlorobenzene, and 0.2 L of a 6 mol / L aqueous acetic acid solution were mixed, subjected to freeze-thaw cycle treatment 5 times, sealed under vacuum, heated at 120° C. for 7 h, filtered, and washed 3 times with tetrahydrofuran to obtain an intermediate monomer;
[0045] Step (2) Under a N2 atmosphere, 25 g of the intermediate monomer, 1.3 g of the magnetic kanamycin sulfate prepared in Example 1, 12 g of 3-mercapto-2-butanone, and 1 mL of benzyltrifluoromethane were mixed and stirred at 90°C for 5 h. The mixture was filtered, and the precipitate was washed five times with tetrahydrofuran. The template kanamycin sulfate was then eluted from the precipitate with a methanol-acetic acid mixture with a volume ratio of 9:1. The mixture was vacuum dried at 70°C for 1 h to obtain an adsorption material.
[0046] Example 4
[0047] See Figure 1 As shown, this embodiment discloses a method for preparing an adsorption material for aminoglycoside antibiotics, comprising the following steps:
[0048] Step (1) 88 g of 2,5-divinyl-1,4-benzenedicarboxaldehyde, 56 g of 1,3,5-tris(4-aminophenyl)benzene, 2 L of 1-butanol, 2 L of 1,2-dichlorobenzene and 0.4 L of a 6 mol / L aqueous acetic acid solution were mixed, subjected to freeze-thaw cycle treatment three times, sealed under vacuum, heated at 80° C. for 5 h, filtered, and washed with tetrahydrofuran five times to obtain an intermediate monomer;
[0049] Step (2) Under a N2 atmosphere, 50 g of the intermediate monomer, 0.6 g of the magnetic amikacin sulfate prepared in Example 1, 25.1 g of 3-mercapto-2-butanone, and 2 mL of benztrifluoromethane were mixed, stirred at 70°C for 7 h, filtered, and the precipitate was washed three times with tetrahydrofuran. The template amikacin sulfate was then eluted from the precipitate with a methanol-acetic acid mixture with a volume ratio of 9:1. The adsorption material was obtained after vacuum drying at 50°C for 3 h.
[0050] Example 5
[0051] See Figure 1 As shown, this embodiment discloses a method for preparing an adsorption material for aminoglycoside antibiotics, comprising the following steps:
[0052] Step (1) 50 g of 2,5-divinyl-1,4-benzenedicarboxaldehyde, 62 g of 1,3,5-tris(4-aminophenyl)benzene, 1.8 L of 1-butanol, 1.2 L of 1,2-dichlorobenzene and 0.25 L of a 6 mol / L aqueous acetic acid solution were mixed, subjected to freeze-thaw cycle treatment 5 times, sealed under vacuum, heated at 90° C. for 5.5 h, filtered, and washed with tetrahydrofuran 3 times to obtain an intermediate monomer;
[0053] Step (2) Under a nitrogen atmosphere, 30 g of the intermediate monomer, 1.1 g of the magnetic neomycin sulfate prepared in Example 1, 23 g of 3-mercapto-2-butanone, and 1.7 mL of benztrifluoromethane were mixed and stirred at 85° C. for 6.2 h. The mixture was filtered, and the precipitate was washed three times with tetrahydrofuran. The template streptomycin sulfate was eluted from the precipitate with a methanol-acetic acid mixture with a volume ratio of 9:1. The mixture was vacuum dried at 65° C. for 2.2 h to obtain an adsorption material.
[0054] Example 6
[0055] See Figure 1 As shown, this embodiment discloses a method for preparing an adsorption material for aminoglycoside antibiotics, comprising the following steps:
[0056] Step (1) 77 g of 2,5-divinyl-1,4-benzenedicarboxaldehyde, 98 g of 1,3,5-tris(4-aminophenyl)benzene, 1.2 L of 1-butanol, 1.6 L of 1,2-dichlorobenzene and 0.25 L of a 6 mol / L aqueous acetic acid solution were mixed, subjected to freeze-thaw cycle treatment 4 times, sealed under vacuum, heated at 105° C. for 7 h, filtered, and washed with tetrahydrofuran 5 times to obtain an intermediate monomer;
[0057] Step (2) Under a N2 atmosphere, 44 g of the intermediate monomer, 0.8 g of the magnetic streptomycin sulfate prepared in Example 1, 16 g of 3-mercapto-2-butanone, and 1.5 mL of benztrifluoromethane were mixed, stirred at 80°C for 6 h, filtered, and the precipitate was washed four times with tetrahydrofuran. The template streptomycin sulfate was eluted from the precipitate with a methanol-acetic acid mixture with a volume ratio of 9:1. The adsorption material was obtained after vacuum drying at 60°C for 1.5 h.
[0058] Example 7
[0059] See Figure 1 As shown, this embodiment discloses a method for preparing an adsorption material for aminoglycoside antibiotics, comprising the following steps:
[0060] Step (1) 72 g of 2,5-divinyl-1,4-benzenedicarboxaldehyde, 101 g of 1,3,5-tris(4-aminophenyl)benzene, 1.5 L of 1-butanol, 1.3 L of 1,2-dichlorobenzene, and 1.35 L of a 6 mol / L aqueous acetic acid solution were mixed, subjected to freeze-thaw cycle treatment three times, sealed under vacuum, heated at 110° C. for 5.2 h, filtered, and washed three times with tetrahydrofuran to obtain an intermediate monomer;
[0061] Step (2) Under a N2 atmosphere, 32 g of the intermediate monomer, 0.8 g of the magnetic gentamicin sulfate prepared in Example 1, 15 g of 3-mercapto-2-butanone, and 1.7 mL of benztrifluoromethane were mixed, stirred at 75°C for 7 h, filtered, and the precipitate was washed five times with tetrahydrofuran. The template gentamicin sulfate was then eluted from the precipitate with a methanol-acetic acid mixture with a volume ratio of 9:1. The adsorption material was obtained after vacuum drying at 70°C for 2.5 h.
[0062] Comparative Example 1
[0063] Comparative Example 1 Compared with Example 2, in the process of preparing the adsorption material in Comparative Example 1, no magnetic template was added, and other conditions remained unchanged.
[0064] Comparative Example 2
[0065] Comparative Example 2 Compared with Example 2, in the process of preparing the adsorption material in Comparative Example 2, no 3-mercapto-2-butanone was added, and other conditions remained unchanged.
[0066] Experimental example
[0067] The properties of the adsorption materials prepared in Examples 2-7 and Comparative Examples 1-2 were tested.
[0068] 1. Specific surface area test
[0069] The test method refers to GB / T 19587-2017 Determination of Specific Surface Area of Solid Substances by Gas Adsorption BET Method, testing instrument: Micromeritics 2020 Plus series, test data are shown in Table 1.
[0070] The test results are shown in Table 1:
[0071] Table 1
[0072] <![CDATA[Specific surface area (m 2 / g)]]> Example 2 581 Example 3 569 Example 4 576 Example 5 572 Example 6 573 Example 7 576 Comparative Example 1 325 Comparative Example 2 387
[0073] The test results in Table 1 indicate that the adsorbent materials prepared in Examples 2-7 of the present invention have a good specific surface area. A comparison between Comparative Example 1 and Examples 2-7 shows that the addition of a magnetic template can increase the specific surface area of the adsorbent material; a comparison between Comparative Example 2 and Examples 2-7 shows that the addition of 3-mercapto-2-butanone can also increase the specific surface area of the adsorbent material.
[0074] 2. Adsorption rate test
[0075] A 0.1 μg / mL mixture of six aminoglycoside antibiotics (tocopherol succinate, kanamycin sulfate, amikacin sulfate, neomycin sulfate, streptomycin sulfate, and gentamicin sulfate) was added to 1.0 mL of ambient water. The solution was diluted to 10.0 mL in a 15.0 mL screw-capped white vial, and 20.0 mg of the synthesized adsorbent was added. The mixture was stirred at 60°C for 30 minutes. After adsorption was complete, the adsorbent and solution were magnetically separated, and the supernatant was discarded. Then, 1 mL of 2% formic acid aqueous solution was added to the screw-capped white vial as a desorbent and stirred at 10°C for 30 minutes. After the target analyte was desorbed from the adsorbent surface, magnetic separation was performed, and the supernatant was collected and filtered. The desorbed solution was analyzed using high-performance liquid chromatography-tandem mass spectrometry.
[0076] The test results are shown in Table 2:
[0077] Table 2
[0078]
[0079] The test results in Table 2 indicate that the adsorbent materials prepared in Examples 2-7 of the present invention have a good specific surface area. A comparison between Comparative Example 1 and Examples 2-7 shows that the addition of a magnetic template can improve the recovery rate of aminoglycosides in the adsorbent material; and a comparison between Comparative Example 2 and Examples 2-7 shows that the addition of 3-mercapto-2-butanone can improve the recovery rate of aminoglycosides in the adsorbent material.
[0080] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.
[0081] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to specific embodiments. Obviously, many modifications and variations are possible based on the contents of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.
Claims
1. A method for preparing an adsorption material for aminoglycoside antibiotics, characterized in that: The following steps are involved: Step (1) mixing a functional monomer, a cross-linking agent, 1-butanol, 1,2-dichlorobenzene and an acetic acid aqueous solution, subjecting the mixture to a freeze-thaw cycle, sealing, heating, filtering and washing to obtain an intermediate monomer; the functional monomer is 2,5-divinyl-1,4-benzenedicarboxaldehyde; the cross-linking agent is 1,3,5-tris(4-aminophenyl)benzene; Step (2) under N2 atmosphere, the intermediate monomer, magnetic template, 3-mercapto-2-butanone and benzyltrifluoromethane are mixed, stirred, filtered, washed, the template is eluted, and vacuum dried to obtain an adsorption material; The method for preparing the magnetic template comprises the following steps: S1: 1-2 g of Fe3O4 nanoparticles were added to 500-1000 mL of anhydrous ethanol and ultrasonicated for 15-20 min. 10-20 mL of ethyl silicate was then added dropwise, stirred for 1-3 h, and centrifuged at 9000-11000 r / min for 10-20 min. The centrifuged solid was washed 3-5 times with deionized water until the pH was neutral, and dried with activated silica at 20-24 ° C for 12-36 h to obtain core-shell Fe3O4; S2: Mix 0.2-0.4 g core-shell Fe3O4, 40-80 mL deionized water, 160-320 mL ethanol and 1.5-3 mL 25 v / v% ammonia water, ultrasonically treat for 25-35 min, mechanically stir at 150-250 r / min at 20-30 ° C for 25-30 min, then add 0.5-1.1 g template molecule, mechanically stir at 150-250 r / min at 20-30 ° C for 50-70 min, then slowly add 2-4 mL ethyl silicate, continue stirring at 150-250 r / min at 20-30 ° C for 60-120 min, separate with an external magnet, and wash alternately with 50-100 mL ethanol and 50-100 mL deionized water for 3-5 times to obtain a magnetic template.
2. The method for preparing an adsorption material for aminoglycoside antibiotics according to claim 1, characterized in that: The template molecule includes at least one of tocopherol succinate, kanamycin sulfate, amikacin sulfate, neomycin sulfate, streptomycin sulfate and gentamicin sulfate.
3. The method for preparing an adsorption material for aminoglycoside antibiotics according to claim 1, characterized in that: In the step (1), the usage ratio of the functional monomer, the cross-linking agent, 1-butanol, 1,2-dichlorobenzene, and the acetic acid aqueous solution is (44-88) g:(56-112) g:(1-2) L:(1-2) L:(0.2-0.4) L.
4. The method for preparing an adsorption material for aminoglycoside antibiotics according to claim 1, characterized in that: In the step (1), the molar concentration of the acetic acid aqueous solution is 6 mol / L; the number of freeze-thaw cycles is 3-5 times; the sealing method is to seal under vacuum; the heating conditions are to heat at 80-120°C and for 5-7 hours; and the washing method is to wash with tetrahydrofuran 3-5 times.
5. The method for preparing an adsorption material for aminoglycoside antibiotics according to claim 1, characterized in that: In the step (2), the usage ratio of the intermediate monomer, the magnetic template, 3-mercapto-2-butanone, and benzenetrifluoromethane is (25-50) g: (0.6-1.3) g: (12-25.1) g: (1-2) mL.
6. The method for preparing an adsorption material for aminoglycoside antibiotics according to claim 1, characterized in that: In the step (2), the stirring treatment conditions are: the stirring treatment temperature is 70-90°C, and the stirring treatment time is 5-7 hours; the washing method is: the precipitate is washed with tetrahydrofuran 3-5 times; the template elution method is: the template is eluted from the precipitate with a methanol-acetic acid mixture with a volume ratio of 9:1; the vacuum drying conditions are: the vacuum drying temperature is 50-70°C, and the vacuum drying time is 1-3 hours.
7. Use of the material obtained by the method for preparing an adsorption material for aminoglycoside antibiotics according to any one of claims 1 to 6, characterized in that: As an extraction adsorbent, it is used for the separation and enrichment of aminoglycoside antibiotics in aqueous systems.
Citation Information
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