CN106243281A - 一种以壳聚糖为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备方法 - Google Patents
一种以壳聚糖为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备方法 Download PDFInfo
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- 229920001661 Chitosan Polymers 0.000 title claims abstract description 21
- 239000000758 substrate Substances 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
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- 229920000344 molecularly imprinted polymer Polymers 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000741 silica gel Substances 0.000 claims abstract description 3
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- 229940056319 ferrosoferric oxide Drugs 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 16
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
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- 238000002955 isolation Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 description 1
- IRLPACMLTUPBCL-KQYNXXCUSA-N 5'-adenylyl sulfate Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OS(O)(=O)=O)[C@@H](O)[C@H]1O IRLPACMLTUPBCL-KQYNXXCUSA-N 0.000 description 1
- WXQDFOGZIYLEGP-UHFFFAOYSA-N C(C(C)C)#N.C(C(C)C)#N.[N] Chemical compound C(C(C)C)#N.C(C(C)C)#N.[N] WXQDFOGZIYLEGP-UHFFFAOYSA-N 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 235000012020 french fries Nutrition 0.000 description 1
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- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
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- 238000003119 immunoblot Methods 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 239000002122 magnetic nanoparticle Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/16—Solid spheres
- C08K7/18—Solid spheres inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/42—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K2201/00—Specific properties of additives
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Abstract
一种以壳聚糖为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备方法属于制备技术,它包括以硅胶为基质的纳米磁珠的制备、分子印迹聚合物包被纳米磁珠。本发明设计新颖,工艺先进,方法独特,用途广。不但解决了丙烯酰胺在传统富集过程中存在的基质干扰、特异性低、成本高等问题,并且实现检测分析快捷方便、样品预处理程序简单、可实现快速检测批量样品,同时易操作,生产成本低,且极具实用性、推广性。
Description
技术领域
本发明涉及的是一种以壳聚糖为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备方法,属于制备技术。
背景技术
丙烯酰胺,一种白色晶体化学物质,极易溶于有机溶剂中。人体可通过消化道、呼吸道、皮肤黏膜等多种途径接触丙烯酰胺,饮水是其中的一条重要接触途径。有报道显示,在一些油炸或烧烤的淀粉类食品,例如薯条、炸土豆片等中检出的丙烯酰胺的含量超过饮水中允许最大限量的500多倍。目前食品中丙烯酰胺的定量检测方法主要是色谱法,特别是色质联用法大大提高了测定的灵敏度和准确度。虽然色谱检测技术在诸多检测方法中最为成熟,得到广泛的认可,但是样品前处理方法依然是限制检测结果的主要因素,传统的前处理方法以液液萃取和固相萃取为主,样品回收率低,基质干扰严重,亟需一种对丙烯酰胺具有较强专一性的样品前处理方法,纳米磁珠具有使用方式简单的优点,分子印迹材料对丙烯酰胺具有高度的选择性吸附,本专利将两者的优点结合研发出一种以硅胶为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备方法,可以应用于含有丙烯酰胺的食品样品的前处理过程,建立高效的丙烯酰胺检测方法。
发明内容
本发明提供一种以壳聚糖为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备方法,可以克服上述困难。
本发明是采用以下技术方案来实现的:一种以壳聚糖为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备方法,它包括以壳聚糖为基质的纳米磁珠的制备、分子印迹聚合物包被纳米磁珠两个步骤。
第一步以壳聚糖为基质的纳米磁珠的制备,先是制备Fe3O4:称取10.0~30.0g七水硫酸亚铁溶解于130.0~140.0ml去离子水中,用磁力搅拌反应浴锅在90℃下反应1h。同时另取1.4~1.8g硝酸钾和10.0~12.0g氢氧化钾溶解于50.0~70.0ml去离子水中,配制好的溶液用恒流泵逐滴(1000μl/min)加入至亚铁离子溶液中。添加完毕继续在90℃下搅拌2h,得黑色浑浊溶液,黑色浑浊即为Fe3O4。
然后是壳聚糖包被Fe3O4:称取1~3g壳聚糖超声溶解于乙酸溶液中,再称取0.1~0.3g Fe3O4磁性纳米粒子加入到100~300ml 6~8mol/L的氢氧化钠溶液中,在磁力搅拌反应浴中搅拌分散。把配制好的壳聚糖溶液逐滴滴加(200μl/min)到亚铁离子溶液中,滴加完毕继续搅拌1h得产物。
第二步分子印迹聚合物包被纳米磁珠,有虚拟印迹和真实印迹两种方法,即分别采用丙酰胺或丙烯酰胺作为模板分子的印迹材料包被纳米磁珠。
(1)采用虚拟印迹方法,即选择丙烯酰胺的结构类似物丙酰胺为模板分子来制备丙烯酰胺分子印迹聚合物(molecularly imprinted polymer,MIP)。称取0.1~0.4g壳聚糖包被Fe3O4纳米磁珠,超声分散于乙腈中,加入模板分子丙酰胺0.01~0.02g,功能单体甲基丙烯酸MAA110.0~112.0μl,交联剂二甲基丙烯酸乙二醇酯EGDMA1100~1300μl,引发剂偶氮二异丁腈AIBN34.0~36.0mg,60℃下搅拌反应12h,磁性分离,乙醇和水洗至中性,用乙醇∶乙酸(8∶1~10∶1)溶液洗脱模板分子。经过冷冻干燥,即得到第一种壳聚糖基质的丙烯酰胺分子印迹纳米磁珠。
(2)采用真实印迹方法:称取0.1~0.4g壳聚糖包被Fe3O4纳米磁珠,超 声分散于乙腈水溶液(乙腈∶水=5∶1~5∶3)中,加入模板分子丙烯酰胺4~6mg,功能单体2-丙烯酰胺基-2-甲基丙磺酸AMPS 0.1~0.3g,交联剂EGDMA1000~1100μl,引发剂AIBN 31.0~32.0mg,通N2 15min排除氧气,将密封好的圆底烧瓶在60℃下搅拌反应17h,磁性分离,乙醇和水洗至中性,用乙醇∶乙酸(9∶1)溶液洗脱模板分子。经过冷冻干燥,即得到第二种壳聚糖基质的丙烯酰胺分子印迹纳米磁珠。
本发明的优点和积极效果:
设计新颖,工艺先进,方法独特,用途广。不但解决了丙烯酰胺在传统富集过程中存在的基质干扰、特异性低、成本高等问题,并且实现检测分析快捷方便、样品预处理程序简单、可实现快速检测批量样品,同时易操作,生产成本低,且极具实用性、推广性。
附图说明
图例为本发明一种以壳聚糖为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备方法的示意流程图。
具体实施方式
由图例给出具体实施例。图例给出的是一种以壳聚糖为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备的工艺流程图,它包括以壳聚糖为基质的纳米磁珠的制备1、分子印迹聚合物包被纳米磁珠2。
Claims (3)
1.一种以壳聚糖为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备方法,它包括以硅胶为基质的纳米磁珠的制备、分子印迹聚合物包被纳米磁珠两个步骤,其特征在于:纳米磁珠和分子印迹技术结合。
2.根据权利要求1所述的一种以壳聚糖为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备工艺,其特征在于:其载体为经壳聚糖包被的四氧化三铁。
3.根据权利要求1所述的一种以壳聚糖为基质,表面覆有丙烯酰胺分子印迹材料的新型纳米磁珠制备工艺,其特征在于:采用丙烯酰胺或丙酰胺分别作为模板分子的印迹材料包被纳米磁珠。
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CN108262488A (zh) * | 2018-01-24 | 2018-07-10 | 浙江农林大学 | 一种金纳米颗粒修饰的纳米磁珠的制备方法 |
CN108262488B (zh) * | 2018-01-24 | 2021-07-06 | 浙江农林大学 | 一种金纳米颗粒修饰的纳米磁珠的制备方法 |
CN110391060A (zh) * | 2019-06-12 | 2019-10-29 | 张裕刚 | 一种磁流体材料的制备方法 |
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