Synthesis And Application Of Polymer-Encapsulated Zirconia-Based Cation Exchange Packing For SPE

Solid phase extraction is a technology for sample preparation in the1970s which hasbeen proved to have many advantages,such as convenient operation,high speed,highconcentration rate, less solvent consumption,easy to realize automation,therefore it has beenwidely used in many fields.Adsorbent is the core of solid phase extraction technique whichshould have high selectivity and strong enrichment ability, good mechanical strength andanti-acid-base capability.More and more attention should be paid in preparation ofmultifunctional composite materials adsorbent is attracting more and more attention toanalytical worker in order to enlarge range of application for solid phase extraction.In thispaper,zirconia powder synthetized was treated by vinyl-silane coupling agent to get vinylmodified zirconia.The SPE packing of cross-linked polystyrene encapsulated zirconia-basedwas synthesized by styrene,divinylbenzene and vinyl-modified zirconia in radicalpolymerization.The polystyrene encapsulated zirconia-based was sulfonated by concentratedsulfuric acid and the cation exchange packing for solid phase extraction was prepared.Thestructure, composition and feature of intermediate reaction product and final product of themeterial were investigated by XRD,FT-IR and SEM was analyzed andmeasured.Polymer-encapsulated zirconia-based cation exchange packing for SPE was used todetermine the content of sulfamerazine and sulfamethazine in water and melamine in milkpowder as adsorbent of solid phase extraction coupled with high performance liquidchromatography. The determination of the content of sulfamerazine and sulfamethazine:Whenthe concentration was in the range of0.005mg/L to0.025mg/L, the linear relation betweenpeak area and concentration of the sulfamerazine and sulfamethazine were good,thecoefficient correlations were0.9904and0.9976separately.The determination of watersample: the contents of sulfamerazine in the lake0.0042mg/L;the contents of sulfamethazinewere0.0034mg/L;the relative standard deviations of sulfamerazine and sulfamethazine were1.06%to3.57%and2.42%to5.05%;recoveries were86.07%to100.3%and90.83%to99.70%;the limits of detective were0.0022mg/L and0.0026mg/L;there were good extractingeffects on self-made-cartridges for solid phase extraction to sulfamerazine andsulfamethazine.The determination of the content of melamine: When the concentration was inthe range of0.2mg/L to1.6mg/L, the linear relation between peak area and concentration of the of melamine was good;the coefficient correlations were0.9987;the relative standarddeviations was5.78%;extraction yield was85.5%;the limits of detective was0.095mg/Kg;there was good adsorptivity on self-made-cartridges for solid phase extraction to melamine.