CN101829550B - Gatifloxacin molecularly imprinted polymer adsorbent and preparation process thereof - Google Patents
Gatifloxacin molecularly imprinted polymer adsorbent and preparation process thereof Download PDFInfo
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- CN101829550B CN101829550B CN2010101797126A CN201010179712A CN101829550B CN 101829550 B CN101829550 B CN 101829550B CN 2010101797126 A CN2010101797126 A CN 2010101797126A CN 201010179712 A CN201010179712 A CN 201010179712A CN 101829550 B CN101829550 B CN 101829550B
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- gatifloxacin
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Abstract
The invention discloses a gatifloxacin molecularly imprinted polymer adsorbent and preparation process thereof. The invention relates to an organic polymer compound, and aims to provide a gatifloxacin molecularly imprinted polymer adsorbent having good selectivity and adsorbability to the gatifloxacin, and preparation process thereof. The technical scheme of the invention is as follows: the gatifloxacin, methylacrylic acid, ethylene glycol dimethacrylate and azodiisobutyronitrile are subject to thermalpolymerization to generate porous spherical high polymer of which the specific surface area is not less than 90m<2>/g. The invention provides the process of the gatifloxacin molecularly imprinted polymer adsorbent described in preparation claim 1, the gatifloxacin, methylacrylic acid, ethylene glycol dimethacrylate and azodiisobutyronitrile are placed in the solvent of acetonitrile or trichloromethane at 50-70 DEG C to thermally initiate the gatifloxacin molecularly imprinted polymer adsorbent. The invention is used for detecting the content of the gatifloxacin.
Description
Technical field:
The present invention relates to a kind of organic high molecular compound, particularly a kind of gatifloxacin molecularly imprinted polymer adsorbent and preparation technology thereof.
Background technology:
Along with the development of livestock breeding industry intensification, the veterinary drug antibiotic is being brought into play more and more important effect aspect the control livestock and poultry infectious disease.The antibiotic extensive large tracts of land of veterinary drug use and exceed standard, no index abuse, though brought bigger economic benefit, also caused multiple negative effect simultaneously to animal husbandry; Exceed standard like antibiotic in meat, egg, fowl, the dairy products; Not only influence the outgoing quality of livestock products, aquaculture is caused great economic loss, also brought serious antibiotic to pollute to breeding water soil simultaneously; Influenced existent environment of people; Finally cause the mankind that antibiotic is produced drug resistance, human health is constituted a serious threat, cause serious economy and environmental pressure.The xacin-series medicine is as widely used veterinary drug antibiotic, and its residue problem in food and environment causes widely day by day to be paid close attention to, and therefore, the analysis of antibiotic residue monitoring is significant to environmental protection and human health.Compare particularity and complexity such as the antibiotic residue analysis has dynamically, trace, the fluctuation of concentration scope is big, sample is complicated, chaff interference is many with the Pharmaceutical Analysis of routine.Therefore, the sample pretreatment before the analyzing and testing more and more becomes the key of analytical technology.Molecularly imprinted polymer is a kind of novel high polymer material with high selectivity that development in recent years is got up; Because it has special molecular recognition performance; Has acid-fast alkali-proof, organic solvent-resistant, Heat stability is good; Advantages such as long service life, therefore at the selective enrichment of samples such as medicine, bioactivator, food and environmental contaminants, separate etc. and to demonstrate application prospects and potentiality aspect the pre-treatment.Yet utilize molecularly imprinted polymer to carry out enrichment to gatifloxacin antibiotic Residual oil thing report is not arranged as yet.
Summary of the invention:
The purpose of this invention is to provide and a kind of gatifloxacin is had selectivity and good gatifloxacin molecularly imprinted polymer adsorbent and the preparation technology thereof of absorption property.Technical scheme of the present invention is; It is characterized in that: it is by gatifloxacin, methacrylic acid, ethylene glycol dimethacrylate and azodiisobutyronitrile; Generate the porous spherical high molecular polymer through heat polymerization, the specific area of this porous spherical high molecular polymer is not less than 90m
2/ g.A kind of technology for preparing the described gatifloxacin molecularly imprinted polymer adsorbent of claim 1; It is characterized in that: the solvent that gatifloxacin, methacrylic acid, ethylene glycol dimethacrylate and azodiisobutyronitrile is placed acetonitrile or chloroform is at 50-70 ℃ of following thermal-initiated polymerization thing gatifloxacin molecularly imprinted polymer adsorbent, and the mol ratio of above-mentioned each composition: gatifloxacin, methacrylic acid: ethylene glycol dimethacrylate: azodiisobutyronitrile is 1: 4～8: ZO: 0.2-1.It is good that the present invention and prior art relatively have gatifloxacin residue concentration effect, thus the remarkable advantage that utilizes conventional detecting instrument and method can carry out detection by quantitative.
Description of drawings:
Accompanying drawing is the Electronic Speculum sketch map of gatifloxacin molecularly imprinted polymer adsorbent of the present invention.
The specific embodiment:
The present invention has following examples:
Embodiment 1
With the gatifloxacin is template molecule; Acetonitrile is a solvent, and methacrylic acid is a function monomer, and ethylene glycol dimethacrylate is a crosslinking agent; Azodiisobutyronitrile is an initator; Template molecule: function monomer: crosslinking agent: the mol ratio of initator is 1: 4: 20: 0.2 (mol ratio), and 60 ℃ of thermal-initiated polymerizations form molecular imprinting microsphere polymer (about 100nm), and this polymer has tangible special absorption property.
Embodiment 2
With the gatifloxacin is template molecule, and chloroform is a solvent, and methacrylic acid is a function monomer; Ethylene glycol dimethacrylate is a crosslinking agent; Azodiisobutyronitrile is an initator, template molecule: function monomer: crosslinking agent: the mol ratio of initator is 1: 4: 20: 0.2 (mol ratio), and 60 ℃ of thermal-initiated polymerizations form molecular imprinting microsphere polymer (about 100nm); This polymer has tangible special absorption property, and maximal absorptive capacity is 246umol/g.
Embodiment 3
With the gatifloxacin is template molecule; Acetonitrile is a solvent, and methacrylic acid is a function monomer, and ethylene glycol dimethacrylate is a crosslinking agent; Azodiisobutyronitrile is an initator; Template molecule: function monomer: crosslinking agent: the mol ratio of initator is 1: 4: 20: 0.6 (mol ratio), and 60 ℃ of thermal-initiated polymerizations form molecular imprinting microsphere polymer (about 100nm), and this polymer has tangible special absorption property.
Embodiment 4
With the gatifloxacin is template molecule, and chloroform is a solvent, and methacrylic acid is a function monomer; Ethylene glycol dimethacrylate is a crosslinking agent; Azodiisobutyronitrile is an initator, template molecule: function monomer: crosslinking agent: the mol ratio of initator is 1: 8: 20: 0.6 (mol ratio), and 60 ℃ of thermal-initiated polymerizations form molecular imprinting microsphere polymer (about 100nm); This polymer has tangible special absorption property, and maximal absorptive capacity is 292umol/g.
Embodiment 5
With the gatifloxacin is template molecule; Acetonitrile is a solvent, and methacrylic acid is a function monomer, and ethylene glycol dimethacrylate is a crosslinking agent; Azodiisobutyronitrile is an initator; Template molecule: function monomer: crosslinking agent: the mol ratio of initator is 1: 4: 20: 0.2 (mol ratio), and 60 ℃ of thermal-initiated polymerizations form molecular imprinting microsphere polymer (about 100nm), and this polymer has tangible special absorption property.
Embodiment 6
With the gatifloxacin is template molecule, and acetonitrile is a solvent, and methacrylic acid is a function monomer; Ethylene glycol dimethacrylate is a crosslinking agent; Azodiisobutyronitrile is an initator, template molecule: function monomer: crosslinking agent: the mol ratio of initator is 1: 6: 20: 1 (mol ratio), and 70 ℃ of thermal-initiated polymerizations form molecular imprinting microsphere polymer (about 100nm); This polymer has tangible special absorption property, and maximal absorptive capacity is 212umol/g.
Embodiment 7
With the gatifloxacin is template molecule, and acetonitrile is a solvent, and methacrylic acid is a function monomer; Left standstill prepolymerization 12 hours in 4 ℃; Ethylene glycol dimethacrylate is a crosslinking agent, and azodiisobutyronitrile is an initator, template molecule: function monomer: crosslinking agent: the mol ratio of initator is 1: 6: 20: 0.2 (mol ratio); 60 ℃ of thermal-initiated polymerizations form molecular imprinting microsphere polymer (about 100nm), and this polymer has tangible special absorption property.
Embodiment 8
With the gatifloxacin is template molecule, and acetonitrile is a solvent, and methacrylic acid is a function monomer; In 25 ℃ of vibration prepolymerizations 12 hours; Ethylene glycol dimethacrylate is a crosslinking agent, and azodiisobutyronitrile is an initator, template molecule: function monomer: crosslinking agent: the mol ratio of initator is 1: 6: 20: 0.2 (mol ratio); 60 ℃ of thermal-initiated polymerizations form molecular imprinting microsphere polymer (about 100nm), and this polymer has tangible special absorption property.
Because the porous spherical high molecular polymerization that heat polymerization of the present invention generates can't confirm specifically that for which kind of material utilize specific area tester (BET) that the specific area of the high molecular polymer of above-mentioned generation is measured, its specific area is 98.08M
2/ gram.
The synthesis mechanism of gatifloxacin molecularly imprinted polymer of the present invention is following:
The technique effect that the present invention produced:
The present invention provides a kind of preparation technology molecular imprinting microsphere polymer simple, with low cost; Said polymer beads is even, and pore capacities is big, and adsorptive selectivity is high; The adsorption rate of polymer is fast.The preparation method is simple, convenient, does not need processes such as loaded down with trivial details grinding, screening, also need not add dispersant, and the trace effect is better.Therefore, the molecular engram microsphere that makes of precipitation polymerization has broad application prospects.Polymer of the present invention and method generally are applied to the processing and the detection of gatifloxacin in environmental sample and the food; Particularly said gatifloxacin molecularly imprinted microsphere polymer with selective absorption performance is analyzed Instrument crosslinking with off-line or online mode and ultraviolet-visible spectrophotometry, liquid chromatogram, liquid chromatography-mass spectrography etc.; Environment and food samples are handled and monitored, will have broad application prospects in the context of detection of trace gatifloxacin antibiotic residue environmental pollution, food security, analytical chemistry etc.
Claims (1)
1. technology for preparing gatifloxacin molecularly imprinted polymer adsorbent; It is characterized in that: be template molecule with the gatifloxacin, acetonitrile is a solvent, and methacrylic acid is a function monomer; Left standstill prepolymerization 12 hours in 4 ℃; Ethylene glycol dimethacrylate is a crosslinking agent, and azodiisobutyronitrile is an initator, template molecule: function monomer: crosslinking agent: the mol ratio of initator is 1: 6: 20: 0.2; The about 100nm microsphere polymer of molecular engram is processed in 60 ℃ of thermal-initiated polymerizations, and this polymer has tangible special absorption property.
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| CN102698720A (en) * | 2012-05-28 | 2012-10-03 | 河海大学 | Method for preparing extraction probe by means of micro-solid phase extraction based on polymer (methacrylic acid-ethyl glycol dimethacrylate) |
| CN102775566B (en) * | 2012-08-15 | 2013-11-13 | 新疆维吾尔自治区分析测试研究院 | Gatifloxacin molecularly imprinted polymer and preparation method of polymer |
| CN104341552B (en) * | 2013-08-02 | 2016-07-06 | 中国科学院大连化学物理研究所 | A kind of fluoroquinolones alternate template molecularly imprinted polymer and application thereof |
| CN109021171B (en) * | 2018-07-26 | 2020-06-12 | 河南师范大学 | Water phase preparation method and application of tylosin tartrate surface molecularly imprinted polymer |
| CN113185655B (en) * | 2021-03-29 | 2023-12-22 | 广西民族大学 | Rosin-based chrysin molecularly imprinted polymer and preparation method and application thereof |
| CN113522253A (en) * | 2021-07-21 | 2021-10-22 | 南京工业大学 | Adsorbent for selectively adsorbing DNA in environment and preparation method thereof |
Citations (3)
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| US6177513B1 (en) * | 1998-08-28 | 2001-01-23 | Toshifumi Takeuchi | Method for evaluating artificial receptors |
| CN101059487A (en) * | 2007-05-31 | 2007-10-24 | 北京望尔生物技术有限公司 | Immunoaffinity chromatography column and its uses in purifying quinolone analogue drug |
| CN101455958A (en) * | 2008-12-04 | 2009-06-17 | 中国农业大学 | Quinolone and sulpha compound extraction method from animal sample and special immuno affinity absorbent |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6177513B1 (en) * | 1998-08-28 | 2001-01-23 | Toshifumi Takeuchi | Method for evaluating artificial receptors |
| CN101059487A (en) * | 2007-05-31 | 2007-10-24 | 北京望尔生物技术有限公司 | Immunoaffinity chromatography column and its uses in purifying quinolone analogue drug |
| CN101455958A (en) * | 2008-12-04 | 2009-06-17 | 中国农业大学 | Quinolone and sulpha compound extraction method from animal sample and special immuno affinity absorbent |
Non-Patent Citations (1)
| Title |
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| 曹玺珉等.环丙沙星分子印迹聚合物的合成及识别性能研究.《化学研究与应用》.2007,第19卷(第12期),第1327页-第1330页. * |
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