Abstract:

A method of simultaneous determination of three organophosphorous flame retardants in textiles by capillary gas chromatograph (GC) combined with nitrogen phosphorus detector (NPD) was developed. The samples were extracted by ultrasonic extraction, filtered by 0.22 μm microporous film and then directly analyzed by GC-NPD. The ultrasonic extraction key factors optimized by the orthogonal design were as follows: the volume ratio of acetone to n-hexane was 2∶8, the extraction time was 40 min and the solvent volume was 35 mL. The linear ranges of tris (2-chloroethyl) phosphate (TCEP), tri-o-cresyl phosphate (TOCP) and tris (2,3-dibromopropyl) phosphate (TRIS) were 0.3758-36.38 μg/mL, 0.3841-38.41 μg/mL and 15.78-1010 μg/mL, respectively, and the detection limits were 0.044 mg/kg, 0.053 mg/kg and 0.82 mg/kg, respectively. Textile samples including cotton, flax, nylon, silk and terylene spiked with different levels of the three flame retardants were employed to investigate the method precision and recovery. For aforementioned analytes, the method precisions were 6.2%, 7.7% and 6.5%, respectively and the method recoveries based on spiked studies were in the range of 83.2%-115.4%. The method is suitable for the determination of three organophosphorous flame retardant residues in textiles in commodity inspection.

Key words: textiles , tri-o-cresyl phosphate, tris (2,3-dibromopropyl) phosphate, tris (2-chloroethyl) phosphate, gas chromatography (GC)