悬浮固化分散液液微萃取-高效液相色谱法测定水体中邻苯二甲酸酯
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摘要
建立了悬浮固化分散液液微萃取(SFO-DLLME)结合高效液相色谱(HPLC)快速测定水样中6种邻苯二甲酸酯(PAEs)的分析方法。通过对影响萃取效率因素的优化,确定了最佳萃取条件:十二烷醇萃取剂20μL、萃取温度60℃、离子强度20 g/L、萃取时间1 min。6种PAEs在2~2 000μg/L范围内呈良好的线性关系,相关系数(r)为0.999 5~0.999 9,检出限(S/N=3)为0.3~0.6μg/L。对自来水、湖水、江水、污水、海水、市售塑料瓶装纯净水和矿泉水进行测定,能检测到部分PAEs。对加标水样进行回收率试验(10、100和1 000μg/L),6种PAEs的回收率为84.9%~94.5%,相对标准偏差为4.1%~6.8%(n=5)。该法环保、简单,可用于实际水样中6种PAEs的检测分析。
A rapid method for the determination of six phthalates(PAEs)in water samples was established by dispersive liquid-liquid microextraction(DLLME)based on solidification of floating organic drop(SFO)coupled with high performance liquid chromatography(HPLC). The influences of the SFO-DLLME parameters on extraction efficiencies were studied. Dodecanol(extraction solvent,20 μL)was added to the water samples(containing 20 g/L NaCl)at 60℃,and the solution was shaken for 1 min. The results showed that the six PAEs were linear in the range of 2-2 000 μg/L with correlation coefficients(r)between 0. 999 5 and 0. 999 9. The limits of detection(S/N = 3)of the six PAEs ranged from 0. 3 to 0. 6 μg/L. The proposed method was applied to the analysis of the seven water samples obtained from different sources(tap water,lake water,river water,waste water,sea water,plastic bottled pure water and mineralwater),and some PAEs were detected. The recoveries of the six PAEs in the spiked water samples were 84. 9%-94. 5%,and relative standard deviations were 4. 1%-6. 8% at three levels of 10,100 and 1 000 μg/L. The method is an environmentally friendly and convenient method for the routine analysis of the PAEs in water samples.
A rapid method for the determination of six phthalates(PAEs)in water samples was established by dispersive liquid-liquid microextraction(DLLME)based on solidification of floating organic drop(SFO)coupled with high performance liquid chromatography(HPLC). The influences of the SFO-DLLME parameters on extraction efficiencies were studied. Dodecanol(extraction solvent,20 μL)was added to the water samples(containing 20 g/L NaCl)at 60℃,and the solution was shaken for 1 min. The results showed that the six PAEs were linear in the range of 2-2 000 μg/L with correlation coefficients(r)between 0. 999 5 and 0. 999 9. The limits of detection(S/N = 3)of the six PAEs ranged from 0. 3 to 0. 6 μg/L. The proposed method was applied to the analysis of the seven water samples obtained from different sources(tap water,lake water,river water,waste water,sea water,plastic bottled pure water and mineralwater),and some PAEs were detected. The recoveries of the six PAEs in the spiked water samples were 84. 9%-94. 5%,and relative standard deviations were 4. 1%-6. 8% at three levels of 10,100 and 1 000 μg/L. The method is an environmentally friendly and convenient method for the routine analysis of the PAEs in water samples.
引文
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[18]Wu X L,Hong H J,Liu X T,et al.Sci Total Environ,2013,444:224
[19]Ye Q,Liu L H,Chen Z B,et al.J Chromatogr A,2014,1329:24
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[22]Sargazi S,Mirzaei R,Rahmani M,et al.J Chromatogr Sci,2015,53:1420