关键词: 加速溶剂萃取, 超高效液相色谱-串联质谱, 涤纶, 禁用偶氮染料

Abstract: A novel method has been developed for the rapid extraction and determination of 22 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 (UPLC-MS/MS). The extract was dried by rotavapor, then through REDOX cracking reaction, and then using ethyl acetate to extract aromatic amines from the reaction liquid. The extract was blowed with N2 to nearly dry, redissolved in the solvent of methanol and water（1∶9，v∶v）.The chromatographic analysis was performed on an acquity UPLC BEH C18 column (100 mm × 2.1 mm，1.7 μm ) by a gradient elution employing of methanol and 0.05% formic acid as a mobile phase. The analytes were detected by electrospray ionization (ESI) tandem mass spectrometry with multiple reaction monitoring (MRM) in positive ion mode. Good linearity (r ＞ 0.99) was observed between 0.01 and 0.2 μg/mL for all compounds. The recoveries and relative standard deviations (RSDs) were checked by spiking untreated samples with the 22 aromatic amines at three levels: 15, 20 and 30 mg /kg. The average recoveries of the 22 aromatic amines were from 33.28 ± 1.83 to 107.14 ± 1.10％. The precision values expressed as RSD were from 0.38 to 10.9％ (n = 6). The limits of detection were from 0.96 to 17 μg/kg, and the limits of quantification were 3.2 to 56.1 μg/kg for the analytes. The results showed that the method can be considered a fast and easy alternative technique with great ruggedness, high degree of automation and good suitability for screening and detecting 22 aromatic amines derived from banned azo colorants in terylene.

Key words: ASE, UPLC-MS∕MS, terylene, banned azo dye