| 柱上衍生气相色谱/质谱法测定纺织品中PFOS |
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| 引用本文： | 刘怡,杨勇,孙明星,林苗. 柱上衍生气相色谱/质谱法测定纺织品中PFOS[J]. 印染, 2012, 38(7): 39-42 |
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| 作者姓名： | 刘怡 杨勇 孙明星 林苗 |
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| 作者单位： | 1. 化学化工与生物工程学院,生态纺织教育部重点实验室,东华大学,上海201620
2. 工业品与原材料检测技术中心,上海出入境检验检疫局,上海200135 |
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| 基金项目： | 上海市质量技术监督局技术性贸易措施应对专项基金 |
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| 摘 要： | 全氟辛基磺酸(PFOS)很难通过常规方法从纺织品中分离、检出.采用超声-微波协同萃取仪提取样品中的PFOS,以四丁基氢氧化铵(TBAH)为衍生化试剂,与PFOS形成铵盐,再在柱上进行衍生化反应,形成PFOS丁酯,进而被气相色谱/质谱(GC/MS)联用仪检出.通过探索最佳衍生化反应条件,确立了柱上衍生GC/MS的检测方法,并对实际纺织样品中PFOS进行分离、检测,结果显示样品中的PFOS含量在0.59～11.27 mg/kg之间,能够满足国际法规对纺织品中PFOS的限量检测要求.
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| 关 键 词： | 测试 气相色谱法 质谱法 全氟辛基磺酸 纺织品 |
Determination of PFOS in textiles by in-port derivatization GC/MS method |
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| LIU Yi , YANG Yong , SUN Ming-xing , LIN Miao. Determination of PFOS in textiles by in-port derivatization GC/MS method[J]. Dyeing and Finishing, 2012, 38(7): 39-42 |
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| Authors: | LIU Yi YANG Yong SUN Ming-xing LIN Miao |
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| Affiliation: | 1 (1.College of Chemistry,Chemical Engineering and Biotechnology,Key Laboratory of Science & Technology of Eco-Textile,Ministry of Education,Donghua University,Shanghai 201620,China;2.Inspection Center of Industrial Product & Raw-Materials,Shanghai Entry-Exit Inspection & Quarantine Bureau,Shanghai 200135,China) |
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| Abstract: | Perfluorooctane sulfonate(PFOS)is difficult to be separated and characterized by conventional techniques.A novel determination method of trace PFOS in textiles have been developed,using in-port derivatization/gas chromatography/mass spectrometry(GC/MS)with ultrasonic-microwave synergistic extraction.Tetrabutylammonium hydroxide(TBAH)is used as a derivative reagent via in situ pyrolytic alkylation reaction which is occurred in the GC injector and finally the derivative of butyl-PFOS is generated.By exploring the best conditions of the derivative reaction,the detecting method of in-port derivatization/ GC/MS is determined.It has been applied to the separation and detection of PFOS in textile samples.The results show that the concentrations of PFOS in the textiles ranged from 0.59 to 11.27 mg/kg.Therefore,this method can meet the demand of relevant international regulations on the limit of detection of PFOS. |
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| Keywords: | testing gas chromatography mass spectrometry perfluorooctane sulfonate textile |
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