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 sec-ondary 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 mx0.25 mmx0.25 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 0.6μg/kg,and the limits of quantification(LOQ)was 2.0μg/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.
dispersed solid-phase extractiongas chromatogeny-tandem mass spectrometryaquatic productorganophosphoric flame retardant
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维普
