轻质分散液液萃取-GC/MS法测定染料中的芳香胺  

Low-density solvent-based dispersive liquid-liquid extraction-GC/MS for determination of harmful aromatic amines in dyestuffs

作　　者：顾娟红[1] 柳艳[1] 李松[1] 李选刚[1] 

机构地区：[1]苏州市出入境检验检疫局,江苏苏州215104

出　　处：《印染》2015年第22期48-51,共4页China Dyeing and Finishing

摘　　要：以密度小于水的轻质溶剂为萃取剂,建立了分散液液萃取-气相色谱质谱法(GC/MS)测定染料中多种有害芳香胺的方法。样品经连二亚硫酸钠在一定条件下还原成芳香胺后,快速注入按一定比例混合的萃取剂(乙酸乙酯)与分散剂(异丙醇)混合溶液获得雾化体系,无需离心,溶液即可澄清、分层,然后取上层有机相进行GC/MS分析测定。试验考察了萃取剂、分散剂种类及体积等因素的影响,确定以4 m L乙酸乙酯为萃取剂,0.5 m L异丙醇为分散剂。结果显示,在1~100 mg/L范围内,各物质呈现良好的线性关系(r^2=0.990 2~0.999 5),各芳香胺的定量限为20 mg/kg,染料基质的加标回收率在70.7%~112.8%,相对标准偏差在2.9%~9.6%。在确定的试验条件下,采用本方法与标准方法没有明显区别。Method of low-density solvent-based dispersive liquid-liquid extraction was developed for the determination of harmful aromatic amines in dyes by gas chromatography-mass spectrometry （GC/MS）. The azo dyes of dye products were reduced by sodium dithionite to form aromatic amines, then, a mix- ture of low-density extraction solvent （ethyl acetate） and dispersive solvent （iso-propyl alcohol） was in- jected into the aqueous sample solution to form an emulsion. No centrifugation was required in this pro- cedure. The upper layer （toluene） was collected and analyzed by GC/MS. Factors affecting the extraction efficiency such as the type and volume of dispersive solvent, extraction solvent were investigated in detail. Under the optimized conditions, the proposed method provided a good linearity in the range of 1 - 100 mg/L （r2=0.990 2 - 0.999 5）. The limits of quantity were 20 mg/kg. The spiked recoveries were be- tween 70.7% -112.8% with the relative standard deviations （RSD） in the range of 2.9% -9.6%. The pro- posed method is fast, efficient and convenient. It has been successfully applied to the determination of AZOs in dyes.

关 键 词：测试 气相色谱法 质谱法 分散液液萃取 染料 禁用芳香胺 

分 类 号：TS107[轻工技术与工程—纺织工程]