Preparation Of Novel Supercrosslinked Polymers And Their Application In The Detection Of Organic Contaminant Residues In Food And Environmental Samples

Organic pollutant residues in food and environmental samples can be harmful to human health,in order to prevent food,environmental pollution and harmful factors on human health,to protect people’s health,to carry out the detection of organic contaminants in food and the environment residues research technology has a positive role and important significance.The matrix of food and environmental samples is complex,with a wide range of residual organic pollutants,most of which are trace or ultra-trace concentrations,which are very difficult to detect directly using instruments.Therefore,it is particularly important to pretreat the samples.Therefore,it is crucial to take effective pretreatment measures to ensure the quality and reliability of the samples.Solid phase extraction(SPE)and magnetic solid extraction(MSPE)techniques are widely used in the analysis of organic contaminants in food and environment because of their advantages of simple operation,small amount of organic solvents,high enrichment multiplicity and environmental protection.The sorbent is the key factor to determine the extraction efficiency of SPE and MSPE techniques.Therefore,the development of new sorbents with high efficiency adsorption capacity is the focus of current research.In this study,three super-crosslinked polymers were synthesized and used as SPE and MSPE adsorbents with high performance liquid chromatography(HPLC)technique to successfully achieve effective enrichment and detection of phenylurea pesticides,chlorophenols and endocrine disruptors in water,honey,apple juice and orange juice.1.In this work,a novel knitting aromatic polymer(KAP)was fabricated for the first time by knitting ferrocene with 1,3,5-tris(bromomethyl)-2,4,6-trimethylbenzene via Friedel-Crafts reaction,and then the KAP was magnetically functionalized with Fe3O4 nanoparticles to produce a magnetic KAP(M-KAP).Combining M-KAP based magnetic solid-phase extraction with high performance liquid chromatography-ultraviolet detection,a simple and sensitive method was developed for simultaneous determination of six benzoylurea insecticides(BUs)in honey and apple juice samples.In the optimized conditions,a good linearity for the BUs existed in the range of 1.67-1000 ng g-1 for honey sample and 0.500-100 ng mL-1 for apple juice sample.The limits of detection were 0.500-1.50 ng g-1 and 0.150-0.400 ng mL-1 for honey and apple juice sample,respectively.Satisfactory recoveries were in the range of 85.5-106%with RSDs ≤8.3%.The developed method demonstrated an excellent practicability for sensitive analysis of the BUs.2.Fabrication of sorbent with large surface area and good adsorption performance for extraction/removal of contaminants has gained significant research interest.In this work,three novel N-rich hypercrosslinked porous polymers(NHCP1,NHCP2,and NHCP3)were facilely developed using Friedel-Crafts alkylation.NHCP1 with the remarkably large surface area(2066 m2 g-1)showed the best adsorption performance for chlorophenol pollutants.A sensitive and simple method was developed by using NHCP1 as sorbent of solid-phase extraction(SPE)to preconcentrate several chlorophenols in honey and water samples,then analysis by HPLC.Under the optimized conditions,the linear ranges were 1.67-1000 ng g-1 for honey and 0.170-100 ng mL-1 for water samples.The detection limits(S/N=3)were 0.500-2.00 ng g-1 and 0.0500-0.100 ng mL-1 respectively.Good method recovery values were 89.3%-111%with the relative standard deviations<9.4%.The proposed extraction/preconcentration and quantitative analysis method provides an affordable and effective alternative for the preconcentration and determination of low levels of chlorophenols in real samples.3.Quantitative analysis of endocrine disrupting chemicals(EDCs)has prominent significance in ensuring human health.Herein,a novel amino-functionalized triazine-based hypercross-linked porous polymer(named DPT-BB)was synthesized for the first time by simple cross-linking of 2,4-diamino-6-phenyl-1,3,5-triazine(DPT)with 4,4’-Bis(chloromethyl)-1,1’-biphenyl(BB).Thanks to the amino functional group(-NH2)and highly crosslinked porous structure,DPT-BB displays remarkable adsorption ability for endocrine disrupting chemicals(EDCs),and adsorption mechanisms mainly involves the hydrogen bond,π-π interaction,hydrophobic interaction and pore adsorption.Thus DPT-BB was applied as sorbent in solid phase extraction cartridge to high efficiently adsorb EDCs from water and orange juice samples prior to subsequent quantitative analysis by high-performance liquid chromatography.Under the optimal conditions,a limit of detection as low as 0.0700-0.200 ng mL-1 for the water sample(0.100-0.270 ng mL-1 for the orange juice sample)was achieved by this DPT-BB based method.After the spiking process,the recovery of the samples reached 83.5-114%and the difference from the standard deviation did not exceed 8.9%.This work not only offers an alternative method for detecting EDCs at trace level,but also provides a viable strategy for the preparation of highly efficient sorbent materials engineered for specific analytes,holding a great application prospective.