色谱

色谱 ›› 2016, Vol. 34 ›› Issue (9): 906-911.DOI: 10.3724/SP.J.1123.2016.05012

• 研究论文 • 上一篇    下一篇

中空纤维液相微萃取-高效液相色谱法测定纺织品中10种含氯苯酚类化合物

高永刚1, 牛增元1, 张艳艳2, 叶曦雯1, 包艳3, 蔡发1, 王新1, 苏杰1, 曲京武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 266003;
    2. 青岛市产品质量监督检验研究院, 山东 青岛 266022;
    3. 中国科学院青岛生物能源与过程研究所, 山东 青岛 266063
  • 收稿日期:2016-05-20 出版日期:2016-09-08 发布日期:2016-08-26
  • 通讯作者: 牛增元
  • 基金资助:

    质检总局科技计划项目（2015IK209）；质检公益性行业专项（201410015-03）.

Determination of 10 chlorinated phenols in textiles by high performance liquid chromatography with hollow fiber liquid phase micro-extraction

GAO Yonggang1, NIU Zengyuan1, ZHANG Yanyan2, YE Xiwen1, BAO Yan3, CAI Fa1, WANG Xin1, SU Jie1, QU Jingwu1   

  1. 1. Technical Center for Inspection & Quarantine of Shandong Entry-Exit Inspection & Quarantine Bureau, Qingdao 266003, China;
    2. Qingdao Testing Research Institute of Product Quality, Qingdao 266022, China;
    3. Qingdao Institute of Biomass Energy and Bioprocess Technology, Chinese Academy of Sciences, Qingdao 266063, China
  • Received:2016-05-20 Online:2016-09-08 Published:2016-08-26
  • Supported by:

    Science and Technology Project of Administration of Quality Supervision, Inspection and Quarantine (No. 2015IK209); Special Funds for Public Welfare Projects of Quality Inspection (No. 201410015-03).

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96

被引次数

4

摘要：

建立了中空纤维液相微萃取-高效液相色谱法测定纺织品中10种含氯苯酚类化合物的方法。系统地优化了影响萃取效率的因素，得到的最佳萃取条件为：萃取溶剂为正己烷，接受相NaOH溶液的浓度为0.10 mol/L，萃取时间为60 min，搅拌速度为600 r/min。在最佳萃取条件下，10种含氯苯酚在0.01～1.00 mg/L范围内线性关系良好（r>0.999），10种含氯苯酚的检出限（信噪比为3）为0.01 mg/kg，富集倍数为95～101。在空白样品中添加0.01、0.05和0.1 mg/kg 3个不同水平的10种含氯苯酚类化合物，其平均回收率为78.8%～105.1%，相对标准偏差为0.3%～7.3%。研究结果表明该方法灵敏度高、简便、准确，可用于纺织品中含氯苯酚类化合物的测定。

关键词: 纺织品, 高效液相色谱, 含氯苯酚类化合物, 液相微萃取, 中空纤维

Abstract:

A method was investigated for the determination of 10 chlorinated phenols in textiles by hollow fiber liquid phase micro-extraction (HF-LPME) coupled with high performance liquid chromatography (HPLC). The experimental conditions of hollow fiber liquid-phase micro-extraction were optimized, such as the nature of organic solvent, the concentration of acceptor phase, stirring rate, extraction time. The optimum extraction conditions were as follows: hexane was used as the organic solvent; the concentration of NaOH solution as acceptor phase was 0.10 mol/L; the stirring rate was 600 r/min; and the extraction time was 60 min. Under the optimal conditions, the calibration curves of the 10 chlorinated phenols were obtained in the range of 0.01-1.00 mg/L (r>0.999); the limits of detection (S/N=3) of the chlorinated phenols were 0.01 mg/kg; and the enrichment factors were 95-101. The proposed method was applied for the determination of the 10 chlorinated phenols in real textile samples. The average recoveries were in the range of 78.8%-105.1% at the spiked levels of 0.01, 0.05 and 0.1 mg/kg; and the relative standard deviations (RSDs) were in the range of 0.3%-7.3%. This method is sensitive, simple, accurate and suitable for the determination of chlorinated phenols in textile samples.

Key words: chlorinated phenols, high performance liquid chromatography (HPLC), hollow fiber (HF), liquid phase micro-extraction (LPME), textiles

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