分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2015年
2期
207-211
,共5页
刘海霞%杨尧霞%马明广%王雪梅%杜新贞
劉海霞%楊堯霞%馬明廣%王雪梅%杜新貞
류해하%양요하%마명엄%왕설매%두신정
金纳米粒子涂层%自组装%固相微萃取%紫外线吸收剂
金納米粒子塗層%自組裝%固相微萃取%紫外線吸收劑
금납미입자도층%자조장%고상미췌취%자외선흡수제
Gold nanoparticles coating%Self-assembly%Solid-phase microextraction%Ultraviolet filters
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)。
以刻蝕不鏽鋼絲為基體,採用化學沉積法在錶麵沉積金納米粒子(AuNPs),脩飾一層1,8-辛二硫醇分子後,再自組裝一層AuNPs,製備瞭高彊度AuNPs塗層固相微萃取( SPME)纖維,併與HPLC聯用,以常用紫外線吸收劑為例,評價瞭AuNPs-SPME纖維的萃取分離性能。噹萃取時間為30 min、溫度為55℃、攪拌速率為800 r/min, pH=7時,萃取效果最好。在優化的萃取條件下,所建立的AuNPs-SPME-HPLC法測定4種紫外吸收劑(2-羥基-4-甲氧基二苯甲酮、2-乙基己基-4-(N,N-二甲氨基)苯甲痠酯、2-乙基己基-4-甲氧基肉桂痠酯和2-乙基己基水楊痠)的線性範圍為0.004~200μg/L,檢齣限為0.43~570 ng/L (S/N=3),相對標準偏差(RSD)在1.9%~4.2%(n=5)之間。河水、廢水處理廠的廢水以及雨水樣品中紫外線吸收劑的加標迴收率在77.9%~108%之間,RSD為3.1%~8.0%(n=5)。
이각식불수강사위기체,채용화학침적법재표면침적금납미입자(AuNPs),수식일층1,8-신이류순분자후,재자조장일층AuNPs,제비료고강도AuNPs도층고상미췌취( SPME)섬유,병여HPLC련용,이상용자외선흡수제위례,평개료AuNPs-SPME섬유적췌취분리성능。당췌취시간위30 min、온도위55℃、교반속솔위800 r/min, pH=7시,췌취효과최호。재우화적췌취조건하,소건립적AuNPs-SPME-HPLC법측정4충자외흡수제(2-간기-4-갑양기이분갑동、2-을기기기-4-(N,N-이갑안기)분갑산지、2-을기기기-4-갑양기육계산지화2-을기기기수양산)적선성범위위0.004~200μg/L,검출한위0.43~570 ng/L (S/N=3),상대표준편차(RSD)재1.9%~4.2%(n=5)지간。하수、폐수처리엄적폐수이급우수양품중자외선흡수제적가표회수솔재77.9%~108%지간,RSD위3.1%~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 ) .