Synthesis And Application Of Myclobutanil Molecular Imprinting Polymers

As a strong suction efficiency, low toxicity and broad-spectrum triazole fungicides,myclobutanil is widely used in fruits, vegetables and traditional chinese medicine to preventand treat herbal rust and leaf spot. The use of myclobutanil can cause residue andaccumulation in crops, therefor it may induce mammal unique neurotoxicity syndrome.Carrying out the analysis to detect residues of myclobutanil in food is important to improveproduct quality and to protect human health.Molecularly Imprinted Polymers (MIP) has an ability to identify specific molecular, ithas the advantages of both the molecular recognition system and the chemical identificationsystem. Introducing MIP into on-line SPE, not only simplifies the procedure of the analysisof biological samples, but also reducing the interference of the other components andreducing the error of quantitative analysis.In this research, myclobutanil was chosen as the template. By improved precipitationpolymerization and based polymerization, packed column and monolithic column wereprepared. Use the column as SPE-column of online SPE HPLC system for the analysis ofcucumber and white peony root.1、Improved precipitation preparation for packed column, performance of charactersand application of packed columnThe optimum preparation conditions of MIP microspheres: nEDMA: nMAA: nmyclobutanil=15:5:1, Vtoluene: Vparaffin=3:2(when nEDMA=12mmol，Vtotal=7.5mL). Under an UVlamp,24h.Scanning electron microscope results showed that the MIP microsphere with adiameter of1~3um, and has a well dispersion. Separation tests showed that on the4.6mm*15mmMIP monolithic column, myclobutanil can be substantially separated from itsstructure analogues, with the mobile phase methanol: water=8:2,0.8mL/min. Frontalchromatography analysis shows that the number of binding sites Lt=85.39mmol/mL,dissociation constant kd=91.38.Online enrichment analysis experiments show that the linear range is0.05-5μg/g,LOD can be reached11ng, recovery between64.04%~71.62%, intraday RSD and interdayRSD were less than18.1%. 2、 Bulk polymerization for monolithic column, performance of characters andapplication of monolithic columnThe optimum preparation conditions of MIP monolithic column: nTRIM: nMAA: nmyclobutanil=15:5:1, Vtoluene: Vdodecane=3:2(when nTRIM=12mmol, Vtotal=7.5mL). Under65℃,24h.Scanning electron microscope results showed that the slice of MIP monolithic columnwith many uniform macroporous. Separation tests showed that on the4.6mm*15mmMIPmonolithic column, myclobutanil can be completely separated from its structure analogues,with the mobile phase methanol: water=7:3,0.8mL/min. Frontal chromatographyanalysis shows that the number of binding sites Lt=182.43mmol/mL, dissociation constantkd=85.41.Online enrichment analysis experiments show that the linear range is0.05-5μg/g,LOD can be reached15ng, recovery between66.46%~79.78%, intraday RSD and interdayRSD were less than16.07%.