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  

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

作　　者：刘慧婷[1] 蒋沁婷 陈笑梅 郑自强 朱晓雨 应义斌[1] 

机构地区：[1]浙江大学生物系统工程与食品科学学院,浙江杭州310029 [2]浙江出入境检验检疫局,浙江杭州310012

出　　处：《纺织学报》2010年第5期97-101,共5页Journal of Textile Research

基　　金：质检公益性行业科研专项项目(10-64)

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-5mmol/L乙酸铵为梯度洗脱淋洗液,13min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0.5～10μg/m2、84.6%～111.8%,检出限为0.5μg/m2,低于欧盟指定针对纺织品1μg/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。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 /m^2,0.5-10 μg /m^2,and 84.6%-111.8%,respectively.It should be pointed out that the limit of detection is 0.5 μg /m^2 by this method which is lower than 1 μg /m^2 regulated for textiles by EU.This method was accurate and swift,which has been successfully applied to analyze 20 real textile samples.

关 键 词：纺织品 全氟化合物 痕量分析 液相色谱串联质谱法 同位素内标法 

分 类 号：TS131.9[轻工技术与工程—纺织材料与纺织品设计]