Preparation of magnetic strong cation exchange resin for the extraction of melamine from egg samples followed by liquid chromatography-tandem mass spectrometry

摘要

In the work, magnetic strong cation exchange (MSCX) resins were prepared using hydrophobic Fe3O4 magnetite as the magnetically susceptible component, styrene and divinylbenzene as polymeric matrix components, acetyl sulfonate as the sulfonation agent. The resins were successfully applied to the extraction of melamine (MEL) from egg samples. The extraction procedure was carried out in a single step by blending and stirring the sample, extraction solvent and the magnetic resins. The MEL was extracted from the sample matrix then adsorbed onto the resins directly through ion-exchange interaction. When the extraction was completed, the resins with adsorbed analyte were easily separated from the sample matrix by applying an appropriate magnetic field. Main factors affecting the extraction of MEL such as the amount of MSCX resins, extraction time, washing and eluting conditions were optimized. The MEL eluted from the resins was determined by liquid chromatography-tandem mass spectrometry. The linearity of quantification obtained by analyzing matrix-matched standards is in the range of 10-1000ngg~(-1). The limit of detection and quantification obtained are 2.6 and 8.8 ng g~(-1), respectively. The relative standard deviations of intra- and inter-day ranging from 1.6% to 6.5% and from 2.1 % to 7.2% are obtained. The recoveries of MEL are in the range of 77.2-99.3%. The proposed method was successfully applied to determine MEL in eggs obtained from different local markets. MEL was detectable with the contents of 43.5 and 234.1 ngg~(-1) in two samples.