摘要
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。
An analytical method using gas chromatography-mass spectrometry( GC-MS) is established for simultaneous determination of 10 kinds of chlorinated phenols in textile. 10 Kinds of chlorinated phenols in samples are extracted by methanol extraction. The extracts in potassium carbonate solution environment are acetylated by acetic anhydride and then extracted by n-hexane. The resulting extracts are separated by using DB-5MS glass capillary column and quantified by mass spectrometry. The results show that the calibration curve for 10 kinds of chlorinated phenols are linear in the range of 1. 0- 200 μg / m L,with linearly dependent coefficient( R^2) higher than 0. 999 6. The detection limits are less than 1. 0 mg / kg. The mean recoveries of 10 kinds of chlorinated phenols are 88. 4%- 103. 6%. The relative standard deviation( n = 6) is 2. 07%- 4. 61%. This method has the advantages such as easy operation,high recovery,high precision and low detection limit,which can be applied to determine the chlorinated phenols in textile. It can also satisfy the requirement for analysis of 10 kinds of phenol compounds in textiles.
出处
《现代化工》
CAS
CSCD
北大核心
2016年第10期193-197,共5页
Modern Chemical Industry