Abstract: An effective method was established for the simultaneous determination of six banned organophosphorous flame retardants in textiles by gas chromatography-tandem mass spectrometry (GC-MS/MS) combined with microwave assisted extraction (MAE). By investigating the extraction efficiency of 12 different extraction solvents for the target analytes, the optimal conditions were that the sample was extracted by microwave assisted extraction using acetone as the solvent at 76 ℃ for 30 min. Then the extract was analyzed by GC-MS/MS in multiple reaction monitoring (MRM) mode, and the concentration of each analyte was calibrated by external standard method. The linear ranges of tris-(1-aziridinyl)phosphine oxide (TEPA), tris-(2-chloroethyl)phosphate (TCEP), tris-(1,3-dichloropropyl)phosphate (TDCP), bis-(2,3-dibromopropyl)phosphate (DDBPP), tri-o-cresyl phosphate (TOCP) and tris-(2,3-dibromopropyl)phosphate (TRIS) were 9.17~366.80, 0.95~75.98, 1.04~83.20, 41.60~832.00, 3.80~75.90, and 40.48~809.60 μg/L, respectively, the correlation coefficients were not less than 0.9975, while the limits of quantification (LOQ) (S/N=10) were 3.0, 0.2, 0.3, 25.0, 2.5 and 29.0 μg/kg, respectively. The spiked recoveries varied from 82.62% to 96.88% with the relative standard deviations of 3.80% to 8.79%. The proposed method was successfully applied to the determination of organophosphorous flame retardants in eight commercial textiles. The experimental results demonstrated that the method developed is simple, rapid, sensitive and accurate, which could satisfy the demand of the analysis of banned organophosphorous flame retardants in textiles.

Key words: gas chromatography-mass spectrometry （GC-MS）, phthalate acid esters, water samples, magnetic multi-walled carbon nanotubes, solid phase extraction （SPE）