高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱筛查和确证纺织品中的致癌染料  

Screening and confirmation of carcinogenic dyes in textiles by high performance liquid chromatography-linear ion trap /Orbitrap high resolution mass spectrometry

作　　者：修晓丽[1,2] 罗忻[2] 牛增元[2] 叶曦雯[2] 汤志旭[2] 李晶莹[1] 王勇为[3] 杜伟[3] 

机构地区：[1]青岛科技大学环境与安全工程学院,山东青岛266042 [2]山东出入境检验检疫局检验检疫技术中心,山东青岛266002 [3]赛默飞世尔科技(中国)有限公司,北京100007

出　　处：《色谱》2013年第10期961-968,共8页Chinese Journal of Chromatography

基　　金：质检公益性行业科研专项项目(201310062);国家质检总局科研项目计划(2011IK037);山东出入境检验检疫局科技项目(SK200994)

摘　　要：建立了高效液相色谱-线性离子阱／静电场轨道阱高分辨质谱（HPLC-LTQ／Orbitrap MS）筛查和确证生态纺织品中致癌染料的方法.样品在水浴（95℃）中用吡啶／水（1／1，v／v）振荡（150r／min）提取．上清液过聚四氟乙烯（PTFE）滤膜后，CAPCELL PAK C18色谱柱（100mm×2．0mm，5μm）分离，以乙腈和5mmol／L乙酸铵水溶液（含0．01％甲酸）、乙腈和5mmol／L乙酸铵水溶液分别作为正、负电喷雾离子化（ESI）模式的色谱流动相梯度洗脱。m／z200～800范围内进行一级质谱全扫描。以准分子离子峰的精确质量数和提取的色谱图峰面积进行筛查分析和定量．以保留时间和数据依赖扫描（data—dependent scan）模式获得的子离子质谱图进行定性确证。9种染料的质量准确度小于5×10^-6（5ppm），线性良好，相关系数大于0．99，方法检出限为0．125～25mg／kg。3个添加水平的回收率范围为62．13％～116．28％，相对标准偏差小于15％.应用该方法检测了棉、涤纶及混纺纤维等20余件纺织品样品中的致癌染料残留。该方法准确、可靠．A method of high performance liquid chromatography-linear ion trap/Orbitrap high resolution mass spectrometry （ HPLC-LTQ/Orbitrap MS） was used to screen and confirm carcinogenic dyes in textiles. The analytes were extracted from textile samples with pyridine/water （1/1, v/v） in a water bath under controlled conditions （95 ℃ 150 r/min）, and then filtered with a 0.22 μm polytetrafluoroetylene （PTFE） membrane. The eluates were separated on a CAPCELL PAK C18 column （ 100 mm× 2.0 mm, 5 μm） using gradient elution with acetonitrile/ 5 mmol/L ammonium acetate aqueous solution containing 0.01% formic acid （in positive mode） and acetonitrile/5 mmol/L ammonium acetate aqueous solution （in negative mode）, and finally detected by HPLC-LTQ/Orbitrap MS in ESI modes. Full scan experiments were performed over the range of m/z 200 - 800. The screening and quantitative analysis were carried out by the accurate mass of quasi-molecular ion and the peak area in extracted chromatogramwith accurate mass, respectively. The confirmatory analysis for target compounds was performed with the retention time and qualitative fragments obtained by data-dependent scan mode. Under the optimal conditions, nine carcinogenic dyes were routinely detected with mass accuracy below 5 × 10^-6（5 ppm）, and good linearities were provided in their respective linear ranges with correlation coefficients higher than 0.99. The limits of detection were in the range of 0. 125 - 25 mg/kg. The average recoveries at three spiked levels were in the range of 52.13% - 116.28% with the relative standard deviations （RSDs） lower than 15%. The proposed method was applied to screen and confirm the nine carcinogenic dyes in textile samples. It is convenient and reliable.

关 键 词：高效液相色谱 线性离子阱-静电场轨道 阱质谱 高分辨质谱 致癌染料 纺织品 

分 类 号：O658[理学—分析化学]