色谱

色谱 ›› 2017, Vol. 35 ›› Issue (4): 453-457.DOI: 10.3724/SP.J.1123.2016.11017

• 研究论文 • 上一篇    下一篇

超临界流体色谱-紫外检测法同时测定混纺地毯中8种致敏性分散染料

楼超艳1, 姜磊2, 段芬3, 王国琴3, 张培敏1, 支明玉4, 朱岩1   

  1. 1. 浙江大学化学系, 浙江 杭州 310000;
    2. 浙江省纺织测试研究院, 浙江 杭州 310013;
    3. 浙江省家具与五金研究所, 浙江 杭州 310013;
    4. 杭州职业技术学院, 浙江 杭州 310018
  • 收稿日期:2016-11-17 出版日期:2017-04-08 发布日期:2013-07-30
  • 通讯作者: 朱岩,E-mail:zhuyan@zju.edu.cn.
  • 基金资助:

    浙江省家具检测技术研究重点实验室资助项目（2016J11）.

Simultaneous determination of eight allergenous disperse dyes in blended carpet by supercritical fluid chromatography-ultraviolet detection

LOU Chaoyan1, JIANG Lei2, DUAN Fen3, WANG Guoqin3, ZHANG Peimin1, ZHI Mingyu4, ZHU Yan1   

  1. 1. Department of Chemistry, Zhejiang University, Hangzhou 310000, China;
    2. Zhejiang Textile Testing Research Institute, Hangzhou 310013, China;
    3. Zhejiang Furniture and Hardware Research Institute, Hangzhou 310013, China;
    4. Hangzhou Vocational & Technical College, Hangzhou 310018, China
  • Received:2016-11-17 Online:2017-04-08 Published:2013-07-30
  • Supported by:

    Key Laboratory of Furniture Inspection Technology of Zhejiang Province (No. 2016J11).

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摘要：

建立了超临界流体色谱-紫外检测同时测定混纺地毯中分散黄1、分散黄49、分散黄9、分散橙37/76、分散红1、分散橙1、分散橙3和分散棕1共8种致敏性分散染料的分析方法。样品在70℃水浴中经甲醇超声萃取30 min后，以超临界态二氧化碳-甲醇（90：10，v/v）为流动相，等度洗脱，在440 nm波长下检测。8种致敏性分散染料在12 min内即可实现分离，其在各自的线性范围内均具有良好的线性关系，相关系数（r2）为0.9992~0.9998，方法的检出限（LOD，S/N=3）为0.05~0.10 mg/L。用该方法分析8种致敏性分散染料，其峰面积的相对标准偏差（RSD）均小于1.2%（n=5）。8种染料在实际样品中的加标回收率为95.6%~104.2%。该方法可以对混纺地毯等纺织品中8种致敏性分散染料进行检测，方法简便、快速、灵敏、选择性高、结果准确，能满足纺织品中致敏性分散染料的检测标准。

关键词: 超临界流体色谱, 混纺地毯, 致敏性分散染料, 紫外检测

Abstract:

An effective analytical method based on supercritical fluid chromatography (SFC) was developed for the simultaneous determination of eight allergenous disperse dyes (disperse yellow 1, disperse yellow 49, disperse yellow 9, disperse orange 37/76, disperse red 1, disperse orange 1, disperse orange 3 and disperse brown 1). Blended carpet samples with various colours were ultrasonically extracted for 30 min with methanol at 70℃. Then the extracts were filtrated by 0.45 μm filters. Under the optimum conditions of supercritical CO2-methanol modifier (90:10, v/v) as mobile phase, 440 nm as UV detection wavelength, the eight allergenous disperse dyes were separated completely within 12 min. The eight allergenous disperse dyes exhibited satisfactory linearity with correlation coefficients (r2) of 0.9992-0.9998. The limits of detection (LOD, S/N=3) were 0.05-0.10 mg/L. The developed method was validated for the determination of the eight allergenous disperse dyes in blended carpets with good spiked recoveries ranged from 95.6% to 104.2%. The relative standard deviations (RSDs) of the peak areas of the eight allergenous disperse dyes were all less than 1.2% (n=5). The method is convenient, rapid, sensitive, accurate, selective, and adaptable to the application for detecting the eight allergenous disperse dyes in blended carpets.

Key words: allergenous disperse dyes, blended carpet, supercritical fluid chromatography (SFC), ultraviolet detection

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