色谱

色谱 ›› 2013, Vol. 31 ›› Issue (10): 961-968.DOI: 10.3724/SP.J.1123.2013.04037

• 研究论文 • 上一篇    下一篇

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

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   

  1. 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
  • 收稿日期:2013-04-21 修回日期:2013-06-19 出版日期:2013-10-28 发布日期:2013-10-08
  • 通讯作者: 牛增元
  • 基金资助:

    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).

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

XIU Xiaoli1,2, LUO Xin2, NIU Zengyuan2, YE Xiwen2, TANG Zhixu2, LI Jingying1, WANG Yongwei3, DU Wei3   

  1. 1. College of Environment and Safety Engineering, Qingdao University of Science and Technology, Qingdao 266042, China;
    2. Technical Center for Inspection and Quarantine of Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China;
    3. Thermo Fisher Scientific (China), Beijing 100007, China
  • Received:2013-04-21 Revised:2013-06-19 Online:2013-10-28 Published:2013-10-08

PDF

201

被引次数

19

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(150 r/min)提取,上清液过聚四氟乙烯(PTFE)滤膜后,CAPCELL PAK C18色谱柱(100 mm×2.0 mm, 5 μm)分离,以乙腈和5 mmol/L乙酸铵水溶液(含0.01%甲酸)、乙腈和5 mmol/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。在m/z 200~800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(5 ppm),线性良好,相关系数大于0.99,方法检出限为0.125~25 mg/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。

关键词: 纺织品, 高分辨质谱, 高效液相色谱, 线性离子阱-静电场轨道阱质谱, 致癌染料

Abstract:

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 chromatogram with 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 62.13%-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.

Key words: carcinogenic dyes, high performance liquid chromatography (HPLC), high-resolution mass spectrometry (HRMS), linear ion trap/Orbitrap mass spectrometer (LTQ/Orbitrap MS), textiles

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