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以1-羟乙基-3-甲基咪唑四氟硼酸(HEMIM[BF4])和1-羟乙基-3-甲基咪唑双三氟甲磺酰亚胺(HEMIM-[N(SO2CF3)2])离子液体为涂层材料,采用溶胶-凝胶方法制备了两种新型的离子液体-羟基硅油(OH-TSO)复合涂层固相微萃取探头,并对溶胶-凝胶反应机理和涂层性能进行了考察.由于阴离子结构不同,两种离子液体-OH-TSO复合涂层的性能也存在一定差异.首先,从表面形貌来看,HEMIM[BF4]-OH-TSO涂层表面孔洞排列更整齐,孔径更小,且大小均一.从热重分析结果来看,HEMIM[N(SO2CF3)2]-OH-TSO涂层具有更高的热稳定性,最高使用温度可以达到360℃.从萃取性能来看,HEMIM[BF4]-OH-TSO涂层对大多数酚类环境雌激素和芳胺的萃取效果明显高于HEMIM[N-(SO2CF3)2]-OH-TSO和未加离子液体的OH-TSO涂层.除此之外,它们还具有较强的抗溶剂冲洗能力,pH应用范围广,重现性好.以HEMIM[N(SO2CF3)2]-OH-TSO涂层为萃取头,采用固相微萃取-气相色谱法测定了实际水体中的芳胺.结果表明,该方法检测限低(6.3～201.3ng/L),线性范围宽(3～4个数量级),重现性好(RSD<7%),准确度高(回收率87.4%～111.5%).
Hydroxyethyl-3-methylimidazolium tetrafluoroborate (HEMIM [BF4]) and 1-hydroxyethyl-3-methylimidazolium bistrifluoromethanesulfonimide (HEMIM- [N (SO2CF3) 2 ]) Ionic liquid as coating material, two new types of solid-phase microextraction probes with hydroxyl-silicone oil (OH-TSO) composite coating were prepared by sol-gel method. The performance of the two ionic liquids -OH-TSO composite coatings are also different due to the different anion structure.Firstly, from the surface topography, HEMIM [BF4] -OH-TSO coating surface pores From the results of TGA analysis, HEMIM [N (SO2CF3) 2] -OH-TSO coating has higher thermal stability and the highest temperature can reach 360 ℃. From the extraction performance point of view, HEMIM [BF4] -OH-TSO coating on most phenolic environmental estrogen and aromatic amine extraction efficiency was significantly higher than the HEMIM [N- (SO2CF3) 2] -OH-TSO and no ion Liquid OH-TSO coating.In addition, they also have a strong anti-solvent washing ability, pH wide range of applications, good reproducibility. With HEMIM [N (SO2CF3) 2] -OH-TSO coating as Extraction head, using solid-phase microextraction - gas phase The results showed that the limit of detection (6.3 ~ 201.3ng / L), wide linear range (3-4 orders of magnitude), good reproducibility (RSD <7%), High accuracy (recovery 87.4% ~ 111.5%).