Determination of aromatic amines in terylene by ASE coupled with UPLC-MS /MS

A novel method has been developed for rapid separation and determination of 22 kinds of aromatic amines derived from banned azo colorants in terylene by accelerated solvent extraction( ASE)with acetone coupled with ultra performance liquid chromatography-tandem mass spectrometry( UPLCMS /MS) in 6 min. The colorants in terylene were extracted by ASE with acetone. The extract was condensed,then subjected to REDOX cracking reaction,and then ethyl acetate was used to extract aromatic amines from the reaction liquid. The extract was blowed with N2to nearly dry,and redissolved in the solvent of methanol and water( 1 /9,v /v). The chromatographic analysis was performed on an Acquity UPLC BEH C18column by a gradient elution employing methanol and 0. 05% formic acid as a mobile phase. The analytes were detected using electrospray ionization( ESI) tandem mass spectrometry with multiple reaction monitoring( MRM) in positive ion mode. The calibration curves showed good linearity in the range of 0. 01- 0. 2 μg /mL for all compounds with the limits of determination( LOD) of0. 96- 17. 0 μg /kg,and the limits of quantification( LOQ) of 3. 2- 56. 1 μg /kg. The recoveries of 22kinds of aromatic amines at the spiked concentration levels of 5. 0,10. 0 and 15. 0 mg /kg ranged from( 33. 28 ±1.83) % to( 107.14 ±1. 10) % with relative standard deviations( RSDs) of 0.38%-10.9%( n =6).