涤纶中致癌芳香胺的加速溶剂萃取－UPLC-MS/MS快速测定

利用加速溶剂萃取结合超高效液相色谱-串联质谱（UPLC-MS∕MS）技术，建立了一种能在6min内快速分离和测定涤纶中禁用偶氮染色剂可分解出的22种致癌芳香胺的方法。样品经丙酮加速溶剂萃取、浓缩，再经氧化-还原裂解反应，用乙酸乙酯萃取反应液中的芳香胺，再将萃取液用N2吹至近干，用甲醇-水溶液（1∶9，v∶v）溶解定容，采用Acquity UPLC BEH C18柱（100 mm × 2.1 mm，1.7 μm）分离，以甲醇-0.05%甲酸溶液为流动相，梯度洗脱，电喷雾正离子模式多反应监测，外标法定量。该方法在0.01～0.2 μg/mL范围内线性关系良好（γ＞0.99），在添加浓度为15 ～ 30 mg/kg水平内，平均回收率范围为33.28 ± 1.83～ 107.14 ± 1.10 ％，相对标准偏差（RSD）为0.38 ～ 10.9％，方法检出限（LOD）为0.96 ～ 17 μg/kg，方法定量限（LOQ）为3.2 ～ 56.1 μg/kg。本方法样品前处理自动化程度高，操作过程简便快速，重复性好，能满足涤纶中的可分解出致癌芳香胺的禁用偶氮染色剂的快速筛选与测定。

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

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.