A simple magnetic solid-phase extraction method based on magnetite/graphene oxide nanocomposite for pre-concentration and determination of melamine by high-performance liquid chromatography.

Abstract

In this study, a clean and simple magnetic solid-phase extraction (MSPE) procedure using magnetite/graphene oxide nanocomposite as an adsorbent was developed for melamine separation and preconcentration from water and dairy products. After synthesis and characterization of the adsorbent, adsorption isotherms and kinetic studies of the adsorption were carried out. The analyte quantification was performed by reversed phase high-performance liquid chromatography after elution of the preconcentrated analytes from the adsorbent surface. Several factors affecting the extraction/preconcentration procedure such as pH, adsorbent amount, extraction time, sample volume, type, and volume of eluent were investigated. The optimizing of some important parameters was assessed by employing a response surface method. The constructed calibration curve in the optimized conditions is linear in the working range of 0.10-100μgL-1 with a correlation coefficient of 0.9999. The detection limit, limit of quantification, and enrichment factor are 0.03μgL-1, 0.10μgL-1, and 500, respectively. The melamine relative recoveries from different real samples are between 97.20 and 103.10% with relative standard deviations of 1.07-4.98%.