气相色谱-质谱法测定纺织品中17种酚类化合物

纺织学报 ›› 2012, Vol. 33 ›› Issue (11): 91-96.

气相色谱-质谱法测定纺织品中17种酚类化合物

韩超¹ 沈浩² 李舟¹ 刘鸿鹏² 周强² 沈燕³

1. 温州出入境检验检疫局
2. 必维申美商品检测（上海）有限公司温州分公司
3. 温州大学化学与材料工程学院

收稿日期:2011-11-25 修回日期:2012-07-27 出版日期:2012-11-15 发布日期:2012-11-20
通讯作者: 沈燕 E-mail:shenyan@wzu.edu.cn

Determination of 17 phenols in textiles by gas chromatography-mass spectrometry

Received:2011-11-25 Revised:2012-07-27 Online:2012-11-15 Published:2012-11-20

摘要/Abstract

摘要： 为了解决同时测定纺织品中多种酚类化合物的问题，建立了气相色谱-质谱法(GC-MS)同时测定纺织品中17种酚类化合物的分析方法。样品用氢氧化钾溶液(2 mol/L)超声提取，将提取溶液与乙酸酐衍生化反应。衍生产物经正己烷提取后，采用GC-MS检测，选择离子模式(SIM)扫描，内标法定量分析。该方法在0.05~0.5 μg/mL范围内呈良好的线性关系，相关系数(r2)≥0.9990；方法的定量限为0.05 mg/kg，平均回收率为89.3% ~ 117.6 %，相对标准偏差小于9.3 %。实验结果表明该方法准确、灵敏，可用于纺织品中17种酚类化合物的分析测定。

关键词: 气相色谱-质谱, 氯酚, 纺织品, 乙酰化

Abstract: To solve the problem of simultaneous determination of multiple phenols in textiles, a method for the determination of 17 phenols in textiles was developed by gas chromatography-mass spectrometry (GC-MS). The sample was extracted with potassium hydroxide (2 mol/L) by ultrasonic; the extract was reacted with acetic anhydride. The derivative was extracted by hexane and determined by GC-MS. Data were acquired in the selected ion monitoring (SIM) mode and quantified by internal standard method. Good linearity was obtained at the mass concentration range of 0.05~0.5 μg/mL with a correlation coefficient (r2) above 0.9990. The limits of quantification (LOQs) were 0.05 mg/kg, the average recoveries were in the range of 89.3%~117.6 % for 17 phenols with the relative standard deviations below 9.3 %. This method is accurate and sensitive, and it is suitable for the analysis of 17 phenols in textiles.

Key words: gas chromatography-mass, apectrometry, phenols, textiles, acetylation

韩超沈浩李舟刘鸿鹏周强沈燕 . 气相色谱-质谱法测定纺织品中17种酚类化合物[J]. 纺织学报, 2012, 33(11): 91-96.

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