纺织学报 ›› 2010, Vol. 31 ›› Issue (5): 97-101.

• 染整与化学品 • 上一篇    下一篇

基于液相色谱-串联质谱法的纺织品中痕量全氟化合物的测定

刘慧婷1;蒋沁婷2;陈笑梅2;郑自强2;朱晓雨2;应义斌1   

  1. 1. 浙江大学生物系统工程与食品科学学院2. 浙江出入境检验检疫局
  • 收稿日期:2009-05-18 修回日期:2009-09-11 出版日期:2010-05-15 发布日期:2010-05-15
  • 通讯作者: 应义斌

Trace analysis of perfluorinated compounds in textile goods by LC/MS/MS method

LIU Huiting1; JIANG Qinting2; CHEN Xiaomei2; ZHENG Ziqiang2; ZHU Xiaoyu2; YING Yibin1

  

  1. 1. College of Biosystems Engineering and Food Science, Zhejiang University 2. Zhejiang Entry-Exit Inspection and Quarantine Bureau
  • Received:2009-05-18 Revised:2009-09-11 Online:2010-05-15 Published:2010-05-15
  • Contact: Yibin Ying

摘要:

采用超声法提取纺织品中的全氟化合物。以C18为分析柱,甲醇-5 mmol/L乙酸铵为梯度洗脱淋洗液, 13 min内即可分离全氟己酸(PFHxA),全氟辛酸(PFOA),全氟壬酸(PFNA),全氟癸酸(PFDA),全氟十一酸(PFuDA),全氟十二酸(PFDoA), 全氟丁烷磺酸(PFBS),全氟己烷磺酸(PFHxS),全氟辛烷磺酸(PFOS),全氟癸烷磺酸(PFDS) 10种分析物。以313.1/268.9,412.9/368.9,462.9/418.9,512.7/468.9,562.7/518.9,612.8/568.9,298.8/99,399.2/99,498.8/99,599/99分别对PFHxA,PFOA,PFNA,PFDA,PFuDA,PFDoA,PFBS,PFHxS,PFOS,PFDS进行监控和定量分析。利用同位素内标法进行定量,线性范围和添加回收率分别为0.5~10 µg/m2、84.6%~111.8%,检出限为0.5 µg/m2,低于欧盟指定针对纺织品1 µg/m2 的限定。结果表明,本方法准确、快速,并成功用于20种纺织品实样的检测。

Abstract:

Ultrasonic method was used to extract PFCs from textiles, and the pretreatment process is convenient. The ten kinds of target compounds, i. e. PFHxA,PFOA,PFNA,PFDA,PFuDA,PFDoA,PFBS,PFHxS,PFOS,and PFDS were separated on C18 reversed phase column in 13 min with step methanol-5 mmol/L ammonium acetate as the mobile phase. Monitor and qualitative analysis of PFHxA,PFOA,PFNA,PFDA,PFuDA,PFDoA,PFBS,PFHxS,PFOS,PFDS were undertaken at 313.1/268.9, 412.9/368.9, 462.9/418.9, 512.7/468.9, 562.7/518.9, 612.8/568.9, 298.8/99, 399.2/99, 498.8/99, 599/99 respectively. Isotope-labeled internal standard method was used to carry out such tests as the limit of detection, linear range, and recovery range. The results showed they were 0.5 µg/m2, 0.5 ~ 10 µg/m2, and 84.6% ~ 111.8%, respectively. It should be pointed out that the limit of detection is 0.5 µg/m2 by this method which is lower than 1 µg/m2 regulated for textiles by EU. This method was accurate and swift, which has been successfully applied to analyzing 20 real textile samples.

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