新型萃取材料及相关涂层制备技术是固相微萃取技术发展的重点。本研究在1-羟丙基-3-甲基咪唑-四氟硼酸盐([C3(OH)mim][BF4])和HNO3混合溶液中,通过电化学方法在铂(Pt)丝表面固定新型聚苯胺-离子液体(PANI-IL)涂层。电镜分析表明,离子液体存在时,PANI膜孔结构变均匀、比表面积增大。以芳香胺为模拟物,考察萃取头的顶空固相微萃取(HS SPME)性能。在优化条件下,5种芳香胺的检出限为0.04~0.12μg/L(S/N=3);线性范围为0.15~1000μg/L。同一萃取头萃取5次的相对标准偏差(RSD)小于4.6%;不同萃取头的RSD则在2.4%~9.5%(n=3)之间。与自制聚苯胺(PANI/Pt)及商品化的聚丙烯酸酯(PA)萃取头相比,PANI-IL/Pt萃取头具有更高的萃取率。此外,PANI-IL涂层对苯类化合物亦有较高的萃取能力。萃取头使用120余次后,萃取性能无明显变化,表明萃取头的稳定性好、使用寿命长。
A novel solid phase microextraction coating of polyaniline-ionic liquid(PANI-IL) was prepared by electrodeposition on a Pt wire in aqueous solutions containing ionic liquid [C3(OH)mim] and nitric acid.The resulted coating was more uniform and porous than PANI coating.Taking five aromatic amines as models,the performance of the PANI-IL/Pt fiber was explored.Under the optimized conditions,when they were determined by GC after headspace SPME with the PANI-IL/Pt,the detection limits were 0.04-0.12μg/L(S/N=3) and the linear ranges were 0.15-1000 μg/L.These aromatic amines were determined for five times using a PANI-IL/Pt fiber coupled with GC and the RSD of chromatographic peak areas were smaller than 4.6%;the fiber to fiber RSD was 2.4-9.5% for different aromatic amines.In comparison with PANI/Pt and commercial PA,the PANI-IL/Pt fiber showed higher extraction efficiency and repeatability.It also exhibited high extraction capability to benzene compounds.The PANI-IL/Pt fiber was used for more than 120 times,its extraction efficiency was almost unchanged,exhibiting good stability and long life time.