Simultaneous determination of 6 organophosphoric flame retardants in aquatic products by GC-MS/MS

A method for simultaneous determination of 6 organophosphoric flame retardants in aquatic products was developed by gas chromatogeny- tandem mass spectrometry (GC-MS/MS) with dispersive solid phase extraction (DSPE) as purification method. The samples were extracted with 0.5% formic acid-acetonitrile solution, after salting out and centrifugation, the supernatant was purified with 4 kinds of solid phase extractants: primary secondary amine (PSA), C18, graphitized carbon black (GCB) and silica gel. After nitrogen (N₂) concentration, it was separated by DB-5ms quartz capillary- column chromatography (30 m×0.25 mm×0.25 μm), and quantified by isotope internal standard. The results showed that the 6 organophosphoric flame retardants had good linear relationship in the range of 1.0-50 μg/L (R²>0.999). The average recovery rates of 6 organophosphoric flame retardants were 79.8%-97.4%, the relative standard deviation (RSD) of precision test results was 2.66%-7.98% under the standard addition 2.0 μg/kg, 4.0 μg/kg and 10.0 μg/kg. The limits of detection (LOD) was 0.6 μg/kg, and the limits of quantification (LOQ) was 2.0 μg/kg. The method had the advantages of simple operation, high sensitivity, good accuracy and precision, and could satisfy the determination requirements of 6 kinds of organophosphate ester flame retardants in aquatic products.