Determination of 5 Chlorophenols and o-Phenyphenol in Textiles Using Dispersive Liquid-Liquid Microextraction with Gas Chromatography-Mass Spectrometry
  
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DOI:10.3969/j.issn.1004-4957.年份.月份
KeyWord:dispersive liquid-liquid microextraction  gas chromatography-mass spectrometry  chlorophenol  o-phenyphenol  textiles
  
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顾娟红,柳艳,徐振东,严敏,黄丽娟 苏州出入境检验检疫局
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Abstract:
      A method for the determination of 5 chlorophenols(PCPs) and o-phenyphenol(OPP) in textiles using dispersive liquid-liquid microextraction(DLLME)coupled with gas chromatography-mass spectrometry(GC-MS) was proposed.Some important parameters affecting extraction efficiency,such as kind of extraction and dispersed solvents and their volume,concentration of K2CO3 were investigated.The optimal conditions were as follows:the sample was extracted with 0.15 mol/L K2CO3 solution in ultrasonic bath.Then 5 mL solution was derivatized with 0.1 mL acetic anhydride for 2 min,then extracted with 0.6 mL of isopropanol(as dispersive solvent) and 0.2 mL carbon tetrachloride (as extraction solution) in ultrasonic bath for 3 min,centrifuged for 3 min at a rate of 4 000 r/min.The lower organic phase was injected to analyze by GC-MS.Under the optimum conditions,the calibration curves were linear in the range of 0.001-1 mg/L,with correlation coefficients of 0.999 1-0.999 9.The detection limits(S/N=3) were in the range of 0.5-5 μg/kg.The average recoveries of the spiked samples were in the range of 87.2%-103.7% with relative standard deviations of 2.5%-4.8%.With the advantages of convinience,sensitivity,good recovery and repeatability,the method was suitable for the detection of 5 chlorophenols and o-phenyphenol in textile samples.
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