快速制备镍钛合金固相微萃取纤维及其与高效液相色谱联用测定环境水样中的紫外线吸收剂  

Determination of Ultraviolet Filters in Environmental Water Samples Using Rapidly Prepared NiTi Alloy Based Solid Phase Microextraction Fiber Coupled with High Performance Liquid Chromatography

作　　者：甄琦[1] 金盼霞 张敏[1] 王会菊[1] 王雪梅[1,2] 杜新贞[1,2] ZHEN Qi JIN Pan-xia ZHANG Min WANG Hui-ju WANG Xue-mei DU Xin-zhen(College of Chemistry and Chemical Engineering, Northwest Normal University, Lanzhou 730070, China Key Lab of Bioelectrochemistry ＆ Environmental Analysis of Gansu, Lanzhou 730070, China)

机构地区：[1]西北师范大学化学化工学院,甘肃兰州730070 [2]甘肃省生物电化学与环境分析重点实验室,甘肃兰州730070

出　　处：《分析测试学报》2017年第3期367-371,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(21265019)

摘　　要：以镍钛合金丝为基体,通过酸处理方法制得具有大比表面积的固相微萃取(SPME)纤维氧化物涂层。将其与高效液相色谱联用,研究了氧化物涂层对芳香分析物的萃取性能。结果表明,该纤维对所选择的紫外线吸收剂具有良好的萃取效率和选择性。进一步优化了紫外线吸收剂2-羟基-4-甲氧基二苯甲酮(BP-3)、2-乙基己基-4-甲氧基肉桂酸酯(EHMC)、4-(二甲氨基)苯甲酸-2-乙基己酯(OD-PABA)和2-乙基己基水杨酸酯(EHS)的萃取条件。方法在0.1~300μg·L^(-1)范围内具有良好的线性关系,检出限为0.025~0.097μg·L^(-1),使用单支SPME纤维同日内和隔日内的精密度分别为4.9%~5.8%和5.5%~6.4%,使用不同批次SPME纤维的精密度为6.3%~7.1%。所建立方法已成功用于环境水样中目标紫外线吸收剂的富集分离和测定。该纤维制作快速简单、稳定性高,不同批次制作的重现性好。A new fiber coating with a large specific surface area was prepared by direct acid pretreatment of NiTi alloy wire.The extraction performance of the prepared fiber was evaluated by high performance liquid chromatography（HPLC） using aromatic compounds as model analytes .Good extraction efficiency and selectivity were achieved for different types of ultraviolet filters.The key parameters influencing the extraction efficiency were optimized for 2-hydroxy-4-methoxybenzophenone（BP-3）,2-ethylhexyl p-methoxycinnamate（EHMC）,2-ethylhexyl-4-（dimethylamino）benzoate（OD-PABA） and 2-ethylhexyl 2-hydroxybenzoate（EHS）.Under the optimized conditions,the linearity was obtained in the range of 0.1-300 μg·L^-1.The limits of detection ranged from 0.025 μg·L^-1 to 0.097 μg·L^-1.The intra day and inter day precisions for the proposed method with the single fiber were in the ranges of 4.9%-5.8% and 5.5%-6.4%,respectively.Its fiber-to-fiber reproducibility ranged from 6.3% to 7.1%.The proposed method was successfully applied in the concentration and determination of target UV filters in environmental water samples.The resulting fiber is very stable in SPME procedure,and could be rapidly prepared in a highly reproducible manner.

关 键 词：固相微萃取(SPME) 高效液相色谱(HPLC) 紫外线吸收剂 富集 样品前处理 

分 类 号：O657.72[理学—分析化学] TQ314.257[理学—化学]