镍钛合金表面离子液体掺杂聚苯基吡咯纤维涂层的制备及其对多氯联苯的高效固相微萃取

Fabrication of an Ionic Liquid Doped Polyphenylpyrrole Fiber Coating on NiTi Alloy and Its Highly Efficient Solid Phase Microextraction on Polychlorinated Biphenyls

采用水热法和电沉积法在镍钛(NiTi)合金表面构筑1-丁基-3-甲基咪唑六氟磷酸盐离子液体(IL)掺杂聚苯基吡咯(PPPy)纤维涂层,成功制备了新型IL@PPPy-TiO2/NiOCNSs固相微萃取(SPME)纤维。将该新型纤维与高效液相色谱(HPLC)联用,以多氯联苯(PCBs)、邻苯二甲酸酯(PAEs)、多环芳烃(PAHs)和紫外线(UV)吸收剂为模型分析物评价其萃取性能。结果显示,该纤维对PCBs有较强的萃取选择性和较高的萃取效率。在优化条件下,5种PCBs在一定质量浓度范围内呈良好线性,相关系数r≥0.9986,检出限(LOD)为0.015~0.11μg/L。采用单支纤维在同日和隔日对50μg/LPCBs混合标准溶液进行萃取测定,相对标准偏差(RSD)分别为4.7%~6.1%和5.4%~7.0%,相同方法制备的5支纤维测定的RSD为6.5%~7.7%。实际水样的加标回收率为83.0%~104%,RSD不大于8.6%。所建立的SPME/HPLC法适用于不同环境水样中痕量PCBs的快速萃取和高效测定。

A novel IL@PPPy-TiO2/NiOCNSs solid phase microextraction fiber was successfully fabricated by using1-butyl-3-methylimidazolium hexafluorophosphate ionic liquid (IL ) doped with polyphenylpyrrole (PPPy ) onto the hydrothermally treated NiTi substrate with electrochemical deposition.The uniform and porous nanoparticles were coated on the surface of NiTi alloy.The extraction performance of the fiber was estimated by the combination of high performance liquid chromatography (HPLC )and itself using polychlorinated biphenyls (PCBs ),phthalic acid ester (PAEs ),polycyclic aromatic hydrocarbon (PAHs ) and ultraviolet (UV ) absorbent as model analytes.The novel IL@PPPy-TiO2/NiOCNSs fiber showed good extraction selectivity and high extraction capability toward PCBs in water samples.The effect factors including extraction temperature,stirring rate,extraction time and ionic strength on the extraction efficiency of PCBs were optimized.Under the optimized condition,there were linear relationships for the analytes in certain mass concentration range with correlation coefficients ( r ) not less than 0.998 6.The limits of detection (LOD ) were in the range of 0.015-0.11 μg/L.The intra-day and inter-day relative standard deviations (RSD ) for a single fiber were in the ranges of 4.7 %-6.1 % and 5.4 %-7.0 %,respectively.The fiber-to-fiber reproducibility ( n =5 ) varied from 6.5 % to 7.7 %.Recoveries for 5 PCBs in real water samples ranged from 83.0 % to104 % with RSD not more than 8.6 %.The proposed SPME/HPLC method was successfully applied in the extraction and detection of trace PCBs in different water samples.