可分解致癌芳香胺偶氮染料检测色谱条件优化  

Optimization of Chromatographic Conditions for the Detection of Decomposable Carcinogenic Aromatic Amine Azo Dyes

作　　者：李典典 Li Diandian(China National Quality Supervision&Inspection Centre for Wool Textile,Beijing 100026,China)

机构地区：[1]国家毛纺织产品质量监督检验中心,北京100026

出　　处：《针织工业》2023年第11期72-76,共5页Knitting Industries

摘　　要：以纺织品禁用偶氮染料分解出的24种芳香胺为研究对象,建立一种快速高效的筛选方法。针对纺织品禁用偶氮染料检测常用的GC-MS联用法,以1.0 mL/min柱流量确定进样口温度、离子源温度和质谱接口温度为前提,考查两种色谱柱的分离效果,并对柱温箱程序升温的条件进行优化。试验分别从方法的重现性、方法的线性、检出限和分离度4个方面对优化结果进行验证。结果表明:柱温条件为60℃(保持1.00 min)→280℃(40℃/min)→310℃(30℃/min,保持3.50 min)的色谱条件较为适宜,在此条件下,各芳香胺通过保留时间和定性离子进行定性,同时用定量的碎片离子也可以很好地定量,且分析时间为11.00 min,大大缩短了仪器检测样品的时间,从而很大程度地提高了检测效率。A fast and efficient screening method was established for 24 aromatic amines which were decomposed by textile banned azo dyes.In view of the commonly used GC-MS in the detection of prohibited azo dye in textiles,the separation effect of two kinds of chromatographic column was examined based on the column flow rate of 1.0mL/min,the input gate temperature,the ion source temperature and the mass spectrum interface temperature,and the heating conditions of column temperature box were optimized.This testing verified the optimization results from four aspects including the reproducibility,the linearity,the detection limit and the degree of separation of the method.The results show that it is appropriate when the column temperature condition is 60 ℃(maintaining 1.00min)→280 ℃(40 ℃/min)→310 ℃(30 ℃/min,maintaining 3.50 min).Under this condition,aromatic amines are characterized by retention time and qualitative ions.At the same time,quantitative debris ions can also be well quantified,and the analysis time is 11.00 min,which greatly reduces the time for the instrument to detect the sample,thus greatly improves the detection efficiency.

关 键 词：偶氮染料 气相色谱-质谱联用 色谱柱 程序升温 色谱条件优化 

分 类 号：TS107[轻工技术与工程—纺织工程]