色谱

色谱 ›› 2015, Vol. 33 ›› Issue (10): 1104-1109.DOI: 10.3724/SP.J.1123.2015.04048

• 技术与应用 • 上一篇    下一篇

高效液相色谱-线性离子阱/静电场轨道阱质谱快速筛查确证生态纺织品中22种致敏性分散染料

牛增元1, 罗忻1, 叶曦雯1, 修晓丽1,2, 张丽1,3, 王新1, 陈静1   

  1. 1. 山东出入境检验检疫局检验检疫技术中心, 山东 青岛 266002;
    2. 青岛科技大学环境与安全工程学院, 山东 青岛 266042;
    3. 中国海洋大学化学化工学院, 山东 青岛 266100
  • 收稿日期:2015-04-28 出版日期:2015-10-08 发布日期:2012-05-09
  • 通讯作者: 牛增元
  • 基金资助:

    质检公益性行业科研专项(201310062);国家质检总局科技项目(2013IK015);山东出入境检验检疫局科技项目(SK200994).

Rapid screening and identification of 22 allergenic disperse dyes in ecological textiles by high performance liquid chromatography- linear ion trap/orbitrap mass spectrometry

NIU Zengyuan1, LUO Xin1, YE Xiwen1, XIU Xiaoli1,2, ZHANG Li1,3, WANG Xin1, CHEN Jing1   

  1. 1. Technical Center for Inspection and Quarantine of Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China;
    2. Collage of Environment and Safety Engineering, Qingdao University of Science and Technology, Qingdao 266042, China;
    3. College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266100, China
  • Received:2015-04-28 Online:2015-10-08 Published:2012-05-09

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被引次数

4

摘要：

建立了基于高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱(HPLC-LTQ/Orbitrap MS)快速筛查确证生态纺织品中22种禁用分散染料的分析方法。样品在95 ℃水浴条件下经吡啶/水(1:1, v/v)振荡提取后,以CAPCELL PAK C18色谱柱分离,以乙腈和5 mmol/L乙酸铵(含体积分数为0.01%的甲酸)作为色谱流动相进行梯度洗脱,采用正、负电喷雾(ESI)离子化模式,利用一级母离子的精确质量数和保留时间对22种分散染料进行快速筛查,利用碰撞诱导解离(CID)下得到的二级碎片离子进行确证。22种分散染料在各自浓度范围内线性关系良好(r2> 0.99),方法的定量限(LOQ)为0.125~2.5 mg/kg。除分散黄49外,绝大多数染料在涤纶布、棉涤混纺布两种纺织品基质中的加标回收率在65%~120%之间,相对标准偏差小于15%。应用本方法对涉及多种纤维类型的40余件纺织品样品进行了筛查,其中一个样品检出分散橙37/76。该方法简便、快速,其选择性高,抗干扰性能好,结果准确可靠,可用于纺织品中分散染料的检测。

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

Abstract:

A rapid screening method based on high performance liquid chromatography-linear ion trap/orbitrap high-resolution mass spectrometry (HPLC-LTQ/Orbitrap MS) for 22 disperse dyes in ecological textiles has been established. The target compounds were extracted by pyridine/water (1:1, v/v) by shaking extraction in 90 ℃ water bath. The extracts were then separated by a CAPCELL PAK C18 column (100 mm×2.0 mm, 5 μm) using gradient elution with acetonitrile-5 mmol/L ammonium acetate containing 0.01% (v/v) formic acid as mobile phases, and finally analyzed by HPLC-LTQ/Orbitrap in positive and negative ESI modes. The retention time and accurate mass of parent ion were used for fast screening of 22 disperse dyes, while the confirmatory analysis was obtained by fragments generated by collision-induced dissociation (CID) MS/MS. Target analysis exhibited high mass accuracy (< 5×10-6). Each target showed a good linearity in its own concentration range and the correlation coefficient was higher than 0.99. The LOQs were 0.125-2.5 mg/kg. Except for Disperse Yellow 49, the average recoveries of most disperse dyes at three spiked levels were 65%-120%, and the relative standard deviations (n=6) were less than 15%. The method was applied for screening 40 different kinds of textiles, and Disperse Orange 37/76 was detected in one of them. With high selectivity and strong anti-jamming ability, this method is simple, rapid, accurate, and it can be used for the inspection of disperse dyes in textiles.

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

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