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

 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。

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

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 0.5μg/m2,0.5-10μg/m2, and 84.6%-111.8%, respectively .It should be pointed out that the limit of detection is 0.μ/m2 by this method which is lower than 1μg/m2 regulated for textiles by EU. This method was accurate and swift,which has been successfully applied to analyze 20 real textile samples.