C18-coated stir bar sorptive extraction combined with high performance liquid chromatography–electrospray tandem mass spectrometry for the analysis of sulfonamides in milk and milk powder

Abstract

A simple, rapid, sensitive, inexpensive and less sample consuming method of C18-stir bar sorptive extraction (SBSE)–high performance liquid chromatography (HPLC)–tandem mass spectrometry (MS/MS) was proposed for the determination of six sulfonamides in milk and milk powder samples. C18 silica particles coated stir bar was prepared by adhesion method, and two kinds of adhesive glue, polydimethylsiloxane (PDMS) sol and epoxy glue were tried. It was found that the C18-coated stir bar prepared by PDMS sol as adhesive glue is more robust than that prepared by epoxy glue when liquid desorption was employed, in terms of both lifetime and organic solvent tolerance. The preparation of C18 stir bar was simple with good mechanic strength and the stir bar could be reused for more than 20 times. Granular coating has relatively high specific surface area and is propitious to sorptive extraction based process. Compared to conventional PDMS SBSE coating, C18 coating shows good affinity to the target polar/weak polar sulfonamides. To achieve optimum SBSE extraction performance, several parameters including extraction and desorption time, ionic strength, sample pH and stirring speed were investigated. The detection limits of the proposed method for six sulfonamides were in the range of 0.9–10.5μg/L for milk and 2.7–31.5μg/kg for milk powder. Good linearities were obtained for sulfonamides with the correlation coefficients (R) above 0.9922. Finally, the proposed method was successfully applied to the determination of sulfonamides in milk and milk powder samples and satisfied recoveries of spiked target compounds in real samples were obtained.