衍生-分散液相微萃取/气相色谱-质谱法测定纺织品中的含氯酚及邻苯基苯酚  

Determination of 5 Chlorophenols and o-Phenyphenol in Textiles Using Dispersive Liquid-Liquid Microextraction with Gas Chromatography-Mass Spectrometry

作　　者：顾娟红[1] 柳艳[1] 徐振东[1] 严敏[1] 黄丽娟[1] 

机构地区：[1]苏州出入境检验检疫局,江苏苏州215104

出　　处：《分析测试学报》2013年第9期1112-1116,共5页Journal of Instrumental Analysis

基　　金：江苏出入境检验检疫局科研项目(2013KJ27)

摘　　要：建立了衍生、分散液相微萃取（DLLME）与气相色谱-质谱（GC-MS）联用测定纺织品中5种含氯酚（PCPs）和邻苯基苯酚（OPP）的方法。对影响萃取和富集效率的因素，萃取剂种类及用量、分散剂种类及用量、碳酸钾溶液浓度等条件进行了优化。确定最佳实验条件为：纺织样品用0.15 mol/L的碳酸钾溶液超声提取后定容，取5 mL溶液，加入0.1 mL乙酸酐进行衍生处理2 min后，经0.2 mL四氯化碳 （萃取剂）与0.6 mL异丙醇 （分散剂）混合溶液分散萃取，在4 000 r/min下离心3 min，取下层有机相进行GC-MS分析。在优化实验条件下，5种含氯酚和邻苯基苯酚的线性范围为0.001-1 mg/L，相关系数为0.999 1-0.999 9，检出限（S/N=3）为0.5-5 μg/kg，样品加标回收率为87.2%-103.7%，相对标准偏差为2.5%-4.8%。方法简单、灵敏，回收率和重复性良好，可用于纺织品中5种含氯酚和邻苯基苯酚的测定。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.

关 键 词：分散液相微萃取 气相色谱-质谱 含氯酚 邻苯基苯酚 纺织品 

分 类 号：O657.63[理学—分析化学] O625.312[理学—化学]