碳納米管基磁性復(fù)合材料分離分析食品中農(nóng)藥殘留的研究
本文選題:分子印跡聚合物 + 碳納米管 ; 參考:《東北林業(yè)大學(xué)》2015年碩士論文
【摘要】:磁性技術(shù)具有快速分離的特征,碳納米管擁有超高的比表面積,分子印跡聚合物具有選擇性吸附能力。本文將磁性,碳納米管和分子印跡技術(shù)相結(jié)合得到的復(fù)合材料應(yīng)用于食品分析,用以解決分析復(fù)雜樣品中農(nóng)藥殘留遇到的問題。主要研究內(nèi)容如下:(1)通過在碳納米管上共沉淀Fe304制備出磁性碳納米管(MCNTs),并對所得到的材料進(jìn)行傅里葉紅外,掃描電子顯微鏡,X射線衍射和綜合物性測量儀表征。將MCNTs用于萃取茶葉樣品中擬除蟲菊酯農(nóng)藥(包括百樹菊酯,功夫菊酯和苯氰菊酯)?疾炝溯腿l件如MCNTs用量,振蕩時間,振蕩速率,淋洗條件,洗脫條件。最終將分離出的農(nóng)藥通過高效液相色譜分析檢測。日內(nèi)日間精密度分別為3.5%-6.4%和4.5%-7.3%。在三種加標(biāo)濃度下(0.05,0.5和5 μg·g-1)回收率達(dá)到了82.2%-94.4%。相比于其他傳統(tǒng)的方法,這種方法更加快捷,具有一定的發(fā)展?jié)摿Α?2)以乙酰甲胺磷為模板分子制備了磁性碳納米管基分子印跡聚合物(MMIPs)。采用傅里葉紅外,透射電子顯微鏡以及振動樣品磁強(qiáng)計進(jìn)行表征。并將MMIPs用于分離分析蔬菜(包括卷心菜,菠菜,生菜,韭菜和芹菜)中的乙酰甲胺磷農(nóng)藥。研究了MMIPs對目標(biāo)物的動力學(xué)吸附和識別性能。采用高效液相色譜對乙酰甲胺磷進(jìn)行檢測。在三種不同濃度的加標(biāo)條件下(0.015,0.15和1.5 mg·kg-1)所得到的回收率在89.2%-93.4%之間。日內(nèi)日間相對標(biāo)準(zhǔn)偏差分別為1.1%-5.9%和2.7%-6.4%。與其他方法相比,本實(shí)驗(yàn)的方法更加迅速而且可以選擇性的吸附蔬菜中的乙酰甲胺磷農(nóng)藥。(3)以殘殺威為模板分子,碳納米管為載體,合成了磁性分子印跡聚合物(MMIPs),用來萃取分離水果中的氨基甲酸酯農(nóng)藥(殘殺威,抗蚜威和猛殺威)。研究了萃取過程中MMIPs用量,振蕩時間,振蕩速率,洗脫溶液對回收率的影響。整個吸附解析過程25 min即可完成,MMIPs能夠通過外加磁場很容易的從基質(zhì)中分離出來。對MMIPs進(jìn)行傅里葉紅外,透射電子顯微鏡和振動樣品磁強(qiáng)計表征。MMIPs成功應(yīng)用于萃取分離水果(蘋果,橙子,梨)中的氨基甲酸酯農(nóng)藥。最終由高效液相色譜測定農(nóng)藥含量,加標(biāo)回收率可以達(dá)到90.5%-98.6%。該方法相對于其他方法更加具有選擇性,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.
【學(xué)位授予單位】:東北林業(yè)大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2015
【分類號】:TQ127.11;TB383.1;TS207.53
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