KOH超声萃取/气相色谱—质谱法同时检测纺织品中19种含氯苯酚

Simultaneous determination of nineteen chlorophenols in textiles by gas chromatography-mass spectrometry combined with KOH ultrasonic extraction

针对现有的纺织品中含氯苯酚检测方法存在的不足,采用氢氧化钾(KOH)溶液对纺织品中的含氯苯酚进行超声萃取,建立气相色谱-质谱(GC-MS)同时检测纺织品中19种含氯苯酚的方法。优化了KOH溶液超声萃取条件,在70℃下,用浓度为2.0 mol/L的KOH溶液超声萃取纺织品样品2.0 h,萃取溶液经乙酸酐乙酰化后,生成含氯苯酚乙酸酯,采用正己烷液液萃取目标物。试验结果表明,在质量浓度1~40μg/L内19种含氯苯酚乙酸酯的峰面积与其质量浓度呈良好的线性关系,相关系数均大于0.995,方法检出限为0.006~0.025 mg/kg,定量下限为0.020~0.082 mg/kg。在0.05、0.50和1.00 mg/kg含氯苯酚的加标水平下,其平均回收率为82.7%~113.3%,相对标准偏差(RSD,n=6)均小于15.0%。该方法操作简便、快速、准确,适用于纺织品中多种含氯苯酚的定量检测。

The ultrasonic extraction of chlorophenol in textiles was carried out by potassium hydroxide(KOH)solution because of the shortcomings of the existing detection methods for chlorophenol in textiles.A method based on gas chromatography-mass spectrometry(GC-MS)was established for the simultaneous determination of 19 chlorophenols in textiles.Pretreatment conditions of extraction were optimized.Textile samples were ultrasonically extracted with 2.0 mol/L KOH solution in 2.0 h under 70℃.The solution was acetylated by acetic anhydride to produce chlorinated phenol acetate and the target was extracted by hexane liquid/liquid extraction.The results show that the calibration curves are linear between the peak area and the concentration of 19 chlorophenol acetates in the range of 1-40μg/L,with correlation coefficients greater than 0.995.The limits of detection(LOD)are 0.006-0.025 mg/kg and the limits of quantitation(LOQ)are 0.020-0.082 mg/kg.The average recoveries range from 82.7%to 113.3%at three different spiked levels of 0.05,0.50 and 1.00 mg/kg,respectively,with relative standard deviation(RSD,n=6)less than 15.0%.The method is simple,rapid and accurate,which is suitable for the determination of various chlorophenols in textiles.