以刻蚀不锈钢丝为基体,采用化学沉积法在表面沉积金纳米粒子(AuNPs),修饰一层1,8-辛二硫醇分子后,再自组装一层AuNPs,制备了高强度AuNPs涂层固相微萃取( SPME)纤维,并与HPLC联用,以常用紫外线吸收剂为例,评价了AuNPs-SPME纤维的萃取分离性能。当萃取时间为30 min、温度为55℃、搅拌速率为800 r/min, pH=7时,萃取效果最好。在优化的萃取条件下,所建立的AuNPs-SPME-HPLC法测定4种紫外吸收剂(2-羟基-4-甲氧基二苯甲酮、2-乙基己基-4-(N,N-二甲氨基)苯甲酸酯、2-乙基己基-4-甲氧基肉桂酸酯和2-乙基己基水杨酸)的线性范围为0.004~200μg/L,检出限为0.43~570 ng/L (S/N=3),相对标准偏差(RSD)在1.9%~4.2%(n=5)之间。河水、废水处理厂的废水以及雨水样品中紫外线吸收剂的加标回收率在77.9%~108%之间,RSD为3.1%~8.0%(n=5)。
Self-assembled gold nanoparticles ( AuNPs) coating was fabricated using an etched stainless steel wire as a support on which AuNPs were first deposited, then after modified with mercaptan, another layer of AuNPs was self-assembled. The AuNPs modified stainless steel wire was used in solid phase microextraction (SPME) coupled with high performance liquid chromatography (HPLC) for the determination of ultraviolet ( UV) filters in environmental water. The best extraction efficiencies were achieved within 30 min at 55℃ and at pH 7 with stirring rate of 800 r/min. Under the optimized conditions, the established AuNPs-SPME-HPLC method for the determination of UV filters benzophnone-3 ( BP-3 ) , 2-ethylhexyl-4-( N, N-dimethylamino ) benzoate ( OD-PABA) , 2-ethylhexyl-4-trimethoxycinnamate ( EHMC) and 2-ethylhexyl salicylate ( EHS) was linear in the range of 0. 004-200 μg/L. The limits of detection of the method were 0. 43-570 ng/L ( S/N=3 ) . The relative standard deviation ( RSD ) of AuNPs-SPME-HPLC was 1 . 9%-4 . 2% ( n=5 ) for spiked water samples of 20 μg/L each UV filter. In the case of real water samples analyses, the recoveries of spiked UV filters were 77 . 9%-108% with RSDs of 3 . 1%-8 . 0% ( n=5 ) .