碳纳米管基磁性复合材料分离分析食品中农药残留的研究

发布时间：2018-04-16 12:18

本文选题：分子印迹聚合物 + 碳纳米管　；参考：《东北林业大学》2015年硕士论文

【摘要】：磁性技术具有快速分离的特征,碳纳米管拥有超高的比表面积,分子印迹聚合物具有选择性吸附能力。本文将磁性,碳纳米管和分子印迹技术相结合得到的复合材料应用于食品分析,用以解决分析复杂样品中农药残留遇到的问题。主要研究内容如下：(1)通过在碳纳米管上共沉淀Fe304制备出磁性碳纳米管(MCNTs),并对所得到的材料进行傅里叶红外,扫描电子显微镜,X射线衍射和综合物性测量仪表征。将MCNTs用于萃取茶叶样品中拟除虫菊酯农药(包括百树菊酯,功夫菊酯和苯氰菊酯)。考察了萃取条件如MCNTs用量,振荡时间,振荡速率,淋洗条件,洗脱条件。最终将分离出的农药通过高效液相色谱分析检测。日内日间精密度分别为3.5%-6.4%和4.5%-7.3%。在三种加标浓度下(0.05,0.5和5 μg·g-1)回收率达到了82.2%-94.4%。相比于其他传统的方法,这种方法更加快捷,具有一定的发展潜力。(2)以乙酰甲胺磷为模板分子制备了磁性碳纳米管基分子印迹聚合物(MMIPs)。采用傅里叶红外,透射电子显微镜以及振动样品磁强计进行表征。并将MMIPs用于分离分析蔬菜(包括卷心菜,菠菜,生菜,韭菜和芹菜)中的乙酰甲胺磷农药。研究了MMIPs对目标物的动力学吸附和识别性能。采用高效液相色谱对乙酰甲胺磷进行检测。在三种不同浓度的加标条件下(0.015,0.15和1.5 mg·kg-1)所得到的回收率在89.2%-93.4%之间。日内日间相对标准偏差分别为1.1%-5.9%和2.7%-6.4%。与其他方法相比,本实验的方法更加迅速而且可以选择性的吸附蔬菜中的乙酰甲胺磷农药。(3)以残杀威为模板分子,碳纳米管为载体,合成了磁性分子印迹聚合物(MMIPs),用来萃取分离水果中的氨基甲酸酯农药(残杀威,抗蚜威和猛杀威)。研究了萃取过程中MMIPs用量,振荡时间,振荡速率,洗脱溶液对回收率的影响。整个吸附解析过程25 min即可完成,MMIPs能够通过外加磁场很容易的从基质中分离出来。对MMIPs进行傅里叶红外,透射电子显微镜和振动样品磁强计表征。MMIPs成功应用于萃取分离水果(苹果,橙子,梨)中的氨基甲酸酯农药。最终由高效液相色谱测定农药含量,加标回收率可以达到90.5%-98.6%。该方法相对于其他方法更加具有选择性,也很方便。
[Abstract]:Magnetic technology has the characteristics of rapid separation, carbon nanotubes have high specific surface area, molecularly imprinted polymers have selective adsorption ability.In this paper, the magnetic, carbon nanotubes and molecularly imprinted composite materials are used in food analysis to solve the problem of pesticide residue analysis in complex samples.The main research contents are as follows: (1) Magnetic carbon nanotubes (MCNTs) were prepared by co-precipitation of Fe304 on carbon nanotubes, and the obtained materials were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), X-ray diffraction (SEM) and comprehensive physical properties measurement.MCNTs was used to extract pyrethroid pesticides (including permethrin, kungthrin and cypermethrin) from tea samples.Extraction conditions such as MCNTs dosage, oscillation time, oscillation rate, elution conditions and elution conditions were investigated.Finally, the isolated pesticides were detected by HPLC.The intra-day precision was 3.5% -6.4% and 4.5% -7.3%, respectively.The recoveries of 0. 05 渭 g g g-1 and 0. 05 渭 g g g-1 were 82.2%-94. 4%.Compared with other traditional methods, this method is more rapid and has a certain development potential. 2) Magnetic carbon nanotube-based molecularly imprinted polymer (MMIPsN) was prepared using acephate as template molecule.Fourier transform infrared (FTIR), transmission electron microscope (TEM) and vibrating sample magnetometer were used.MMIPs was used to separate and analyze acephate pesticides in vegetables (including cabbage spinach lettuce leek and celery).The kinetic adsorption and recognition properties of MMIPs to the target were studied.Acetamidophos was detected by high performance liquid chromatography (HPLC).The recoveries of 0.015 ~ 0.15 and 1.5 mg / kg ~ (-1) were in the range of 89.2-93.4%.The relative standard deviations between days were 1.1% -5.9% and 2.7% -6.4%, respectively.Compared with other methods, this method is more rapid and can selectively adsorb acephate pesticide in vegetables. It uses propoxur as template molecule and carbon nanotube as carrier.A magnetic molecularly imprinted polymer (MMIPsN) was synthesized for the extraction and separation of carbamate pesticides (propoxur, aprimicarb, and fenprovir) from fruits.The effects of MMIPs dosage, oscillation time, oscillating rate and elution solution on the recovery were studied.MMIPs can be easily separated from the matrix by an external magnetic field in the whole adsorption and desorption process of 25 min.MMIPs was characterized by Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and vibrating sample magnetometer. MMIPs were successfully used to extract carbamate pesticides from fruits (apple, orange and pear).Finally, the pesticide content was determined by HPLC, and the recoveries reached 90.5-98.6.This method is more selective and convenient than other methods.
【学位授予单位】：东北林业大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TQ127.11;TB383.1;TS207.53

【参考文献】