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建立了气相色谱-质谱法(GC-MS)同时测定纺织品中10种含氯苯酚化合物含量的检测技术。样品中10种含氯苯酚化合物经甲醇萃取,提取液在碳酸钾溶液环境中经乙酸酐乙酰化后以正己烷萃取,最后经DB-5MS型毛细管气相色谱柱分离及质谱定量。结果表明:10种含氯苯酚化合物在1.0~200μg/m L范围内呈良好的线性关系,线性相关系数R~2>0.999 6;检出限均低于1.0 mg/kg;回收率为88.4%~103.6%,相对标准偏差(n=6)为2.07%~4.61%。该方法具有前处理简单,回收率高,精密度好,检出限低等特点,能够满足对纺织品中10种含氯苯酚化合物的分析要求。
A gas chromatography-mass spectrometry (GC-MS) method for the simultaneous determination of ten chlorophenols in textiles was established. Ten kinds of chlorophenols in the sample were extracted by methanol. The extract was acetylated with acetic anhydride in the environment of potassium carbonate solution and extracted with n-hexane. Finally, the compounds were isolated by DB-5MS capillary gas chromatography and quantified by mass spectrometry. The results showed that the 10 chlorophenols showed a good linearity in the range of 1.0 ~ 200μg / m L with a linear correlation coefficient of R ~ 2> 0.999 6 and a detection limit of less than 1.0 mg / kg. The recoveries were 88.4% ~ 103.6%, relative standard deviation (n = 6) was 2.07% ~ 4.61%. The method has the advantages of simple pretreatment, high recovery rate, good precision, low detection limit, and the like, and can meet the requirements for analyzing 10 kinds of chlorophenol compounds in textiles.