超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱鉴别纺织品中禁用芳香胺及其异构体  

Identification of banned aromatic amines and their isomers in textiles by ultra-performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry

作　　者：叶曦雯[1] 彭燕[2] 牛增元[1] 高永刚[1] 罗忻[1] 邹立[2] 周明辉[3] 

机构地区：[1]山东出入境检验检疫局,山东青岛266002 [2]中国海洋大学环境科学与工程学院,山东青岛266100 [3]广东出入境检验检疫局,广东广州510623

出　　处：《色谱》2014年第9期1005-1012,共8页Chinese Journal of Chromatography

基　　金：国家质检公益性行业科研专项基金项目(201310062);"双打"中急需的出入境检验检疫技术方法研究项目(2012104020);国家质检总局科研项目(2013IK015)

摘　　要：针对目前纺织品中禁用偶氮染料检测中的假阳性问题,建立了一套应用超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱（UPLC-LTQ/Orbitrap）同时筛选24种禁用芳香胺及其常见的14种异构体的方法。样品经连二亚硫酸钠还原,叔丁基甲醚提取后,以水/甲醇（9/1,v/v）稀释定容,用ZORBAX SB-C18色谱柱（150 mm×2.1mm,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。38种芳香胺的线性相关系数大于0.99,方法检出限为0.5-5μg/kg。该方法可通过一次实验同时对24种禁用芳香胺及其常见的14种异构体准确定性定量,大大缩短检测周期,实际样品检测也进一步验证了其灵敏性和准确性。A method of ultra-performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry （UPLC-LTQ/Orbitrap MS） was used to screen and confirm 24 banned aromatic amines and their 14 isomers at the same time. The main factors influencing the separation including the column, and the nature of make-up solvent were optimized. Under the optimized experimental conditions, the analytes were reduced to banned aromatic amine with sodium dithionite, extracted by methyl tert-butyl ether and loaded onto a ZORBAX SB-C18 column （ 150 mm×2. 1 mm, 5 μm） with a gradient elution of methanol and 0. 1% formic acid aqueous 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 chro- matogram with accurate mass. The correlation coefficients were higher than 0.99 and the limits of detection were in the range of 0.5-5 μg/kg. The method could screen and confirm the 24 banned aromatic amines and their 14 isomers at the same time. The results were 1. 56 mg/kg of 4-chloroaniline, 0. 34 mg/kg of o-toluidine, and 0.81 mg/kg of 2,6-toluylenediamine with the relative standard deviations ranging from 0.27% to 1.32% in actual samples. The results indicate that the developed method is simple, efficient and precise, and can be a reliable technique for the separation of the 24 banned aromatic amines and their 14 isomers in textile samples.

关 键 词：超高效液相色谱 线性离子阱 静电场轨道阱质谱 高分辨质谱 禁用偶氮染料 同分异构体 纺织品 

分 类 号：O658[理学—分析化学]