皮革和纺织品中重叠峰偶氮染料的气相色谱-串联质谱检测技术

Determination of overlapping peaks of prohibited azo dyes in leather and textiles by gas chromatography-tandem mass spectrometry

建立了气相色谱-串联质谱一次进样同时检测重叠峰偶氮染料的分析方法。皮革和纺织品中的偶氮染料用柠檬酸盐缓冲液提取,再用连二亚硫酸钠将其还原裂解为胺类物质,经液-液萃取、浓缩处理,所得残渣用甲醇溶解,通过VF-5ms色谱柱分离,采用串联质谱的多反应监测模式开设多通道存储子离子信息,进行定性、定量分析。实验结果表明:优化质谱分析条件后,气相色谱-串联质谱可进一步消除杂质干扰,分离共流出组分。大部分芳香胺3种浓度水平的加标回收率(n=6)保持在71%～94%之间,检测限为0.008～0.672μg/mL(S/N=3),相对标准偏差(n=6)小于11%,2～50μg/mL浓度范围内线性相关系数大于0.9917,满足禁用偶氮染料的分析要求。

An effective method for the simultaneous determination of prohibited azo dyes in leather and textiles by gas chromatography-tandem mass spectrometry was developed in this paper. Samples of leather or textiles was extracted with sodium citrate buffer solution, which was defatted, the residue obtained was dissolved with methanol and separated on the VF-5ms column after liquid-liquid extraction and concentration. Azo dyes can be converted into the amines by sodium hydmsulfite, qualitative and quantitative analyses were carried out by applying several channels to observe the information of characteristic fragment ions in multiple reaction monitoring mode. The result shows that this method is simple, rapid, sensitive, linear, accurate, and separated compounds and the interference with background signal were further eliminated after GC-MS/MS analytical condition were optimized. The average recoveries of a majority of aromatic amines in leather and textiles at three levels ranged from 71% to 94 %, the relative standard deviations （ n = 6） were lower than 11%, the limits of detection were between 0.008 and 0.672 μg/mL, the correlation coefficient was above 0. 9917 over the range 2 - 50μg/mL. The method was suitable for the determination of prohibited azo dyes in leather and textiles.