CN106188396A - 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 - Google Patents

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 Download PDF

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CN106188396A
CN106188396A CN201610585476.5A CN201610585476A CN106188396A CN 106188396 A CN106188396 A CN 106188396A CN 201610585476 A CN201610585476 A CN 201610585476A CN 106188396 A CN106188396 A CN 106188396A
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magnetic bead
silica gel
substrate
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丁轲
孙毅蒙
韩涛
陈湘宁
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Beijing University of Agriculture
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Abstract

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

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
技术领域
本发明涉及的是一种以硅胶为基质，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，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，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。
第一步以硅胶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SiO2包被Fe3O4：称取0.2～0.6gFe3O4超声5min分散于10.0～30.0ml0.5～2mol/l HCl溶液中，在磁铁提供的外加磁场作用分离后去离子水洗涤至中性，然后分散于乙醇∶水＝1∶4～1∶6的150ml乙醇溶液中，冰水浴下超声15min。然后添加3～5ml氨水和5～7ml正硅酸乙酯，在冰水浴下再超声振荡2h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 SiO2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，即得到第一种硅胶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 SiO2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EGDMA 1000～1100μl，引发剂AIBN 31.0～32.0mg，通N215min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，即得到第二种硅胶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的工艺流程图，它包括以硅胶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，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工艺，其特征在于：其载体为经二氧化硅包被的四氧化三铁。
3.根据权利要求1所述的一种以硅胶为基质，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。
CN201610585476.5A 2016-07-25 2016-07-25 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 Pending CN106188396A (zh)

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