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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。
A method for the determination of 10 chlorinated phenolic compounds in textiles by hollow fiber liquid phase microextraction and high performance liquid chromatography was established. The optimal extraction conditions were systematically optimized as follows: the extraction solvent was n-hexane, the concentration of NaOH in the receiving phase was 0.10 mol / L, the extraction time was 60 min, and the stirring speed was 600 r / min. Under the optimal extraction conditions, the linearity of 10 chlorophenols in the range of 0.01-1.00 mg / L was good (r> 0.999). The detection limits (signal to noise ratio) of 10 chlorophenols were 0.01 mg / kg, the enrichment factor is 95 ~ 101. The average recoveries of 10 chlorinated phenols were 0.01%, 0.05% and 0.1 mg / kg, respectively. The average recovery was 78.8% -105.1% and the relative standard deviation was 0.3% -7.3%. The results show that the method is sensitive, simple and accurate and can be used for the determination of chlorophenols in textiles.