建立了超高效液相色谱?线性离子阱／静电场轨道阱高分辨质谱（ UPLC?LTQ／Orbitrap MS）同时测定纺织品中24种游离态致癌芳香胺的方法。样品经二氯甲烷超声提取并稀释后，用ZORBAX SB?C18色谱柱（150 mm×2?1 mm，5μm）分离，以0?1％甲酸水溶液和甲醇为流动相，电喷雾正离子（ ESI＋）模式电离，以准分子离子峰的精确质量数和保留时间定性，以提取的色谱图峰面积定量。在0?5～500μg／L范围内，24种芳香胺的线性相关系数（ R2）大于0?99，样品加标回收率为87?8％～105?6％，相对标准偏差为1?6％～3?4％。方法检出限为0?5～1μg／kg。应用本方法检测山东地区进出口含氨纶纺织品样品14个，在5个样品中检出游离态芳香胺4，4′?二氨基二苯甲烷，含量范围为0?21～25?6 mg／kg。
A method of ultra?performance liquid chromatography?linear ion trap/orbitrap high resolution mass spectrometry ( UPLC?LTQ/Orbitrap MS) was used to determine 24 free carcino?genic aromatic amines in textiles. The main factors influencing the method, including the extraction solvent, the extraction temperature and the extraction time, were optimized. Under the optimized experimental conditions, the analytes were extracted by dichloromethane for 10 min and loaded into a ZORBAX SB?C18 column (150 mm×2?1 mm, 5μm) with a gradient elu?tion of methanol and 0?1% aqueous formic acid solution, and finally detected by LTQ/Orbitrap MS. The screening and quantitative analysis were carried out by the accurate mass of quasi?molecular ion and the peak in extracted chromatogram with accurate mass respectively. The correlation coefficients ( R2 ) were higher than 0?99. The recoveries were 87?8%-105?6% with the RSDs were 1?6%-3?4%. The limits of detection were 0?5-1μg/kg, and the limits of quanti?fication were 1?5-3 μg/kg. The proposed method was applied to 14 textile samples containing spandex. 4,4′?Diaminodiphenylmethane was determined in five samples and the contents were 0?21-25?6 mg/kg. The results indicate that the developed method is a simple, efficient, precise and reliable technique for the determination of free carcinogenic aromatic amines in textiles.
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