Development of an on-line matrix solid-phase dispersion/fast liquid chromatography/tandem mass spectrometry system for the rapid and simultaneous determination of 13 sulfonamides in grass carp tissues

摘要

A novel analytical protocol based on interfacing on-line matrix solid-phase dispersion (MSPD) with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for extraction and determination of 13 sulfonamide residues in grass carp tissues. The target analytes were separated on a fused-core C18-silica column with a period of 7min and quantified by a triple-quadrupole linear ion-trap mass spectrometer in positive ion multiple-reaction monitoring (MRM) mode. The proposed method was optimized and validated according to Commission Decision 2002/657/EC. The matrix-matched calibration curves were performed at six concentration levels and good linear relationship (R2=0.993-0.998) was observed within the range of 0.1-100ngmL~(-1). The mean values of relative standard deviation of intra- and inter-day ranging from 1.8% to 7.8% and from 2.8% to 10.3% were obtained, respectively. Moreover, satisfied recoveries (69.0-96.3%) of all studied sulfonamides were demonstrated in different spiked levels, with RSDs≤13.2%. The proposed method has been applied successfully to the analysis of sulfonamides in several grass carp samples, and the results indicated that this novel instrumental coupling was fast, sensitive, reliable and environmental friendly with good prospects.