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  

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

作　　者：高永刚[1] 牛增元[1] 张艳艳 叶曦雯[1] 包艳[3] 蔡发[1] 王新[1] 苏杰[1] 曲京武[1] 

机构地区：[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

出　　处：《色谱》2016年第9期906-911,共6页Chinese Journal of Chromatography

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

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 /k g,富集倍数为9 5 - 1 0 1.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.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 phe-nols 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.

关 键 词：高效液相色谱 中空纤维 液相微萃取 含氯苯酚类化合物 纺织品 

分 类 号：O658[理学—分析化学]