漂浮有机液滴凝固液相微萃取法测定海绵城市水体中痕量拟除虫菊酯类药物
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摘要
目的测定海绵城市水体中痕量联苯菊酯、甲氰菊脂、氯菊酯及溴氰菊酯。方法采用漂浮有机液滴凝固分散液相微萃取技术(SFOD-LPME)与气相色谱相结合,同时采用超声和表面活性剂辅助加快萃取过程,并采用外标法进行分析。结果本实验选择超声时间为1.5 min,超声温度为20℃,萃取剂为十六烷,用量为80μl,表面活性剂吐温20最佳用量为20μl,联苯菊酯、甲氰菊脂、氯菊酯及溴氰菊酯的线性相关系数为0.999 6～0.999 8,线性范围为5～300μg/L,检出限为0.03～0.05μg/L。采用此方法对徐州市区云龙湖水、实验室自来水进行2个浓度的加标回收实验,回收率为95.4%～107.8%,相对标准偏差(RSD)2.74%～6.09%(n=6),检出浓度符合国家标准。结论本方法创新发展前处理技术,使用绿色环保、用量极少的有机溶剂,灵敏度高,回收率和重现性均好。
Objective To detect trace amounts of bifenthrin,fenpropathrin,permethrin,and deltamethrin in urban sponge water.Methods The extraction was carried out by using solidification of floating organic drop liquid-phase micr-extraction(SFOD-LPME) technique combined with gas chromatography method,and was quickened by the assist of ultraphonic method and surfactants.The results were analyzed with external reference method.Results In this experiment,the ultrasonic time was 1.5 min,the ultrasonic temperature was 20 ℃,the extractant was hexadecane,the dosage was 80 μl,and the optimal dosage of surfactant Tween 20 was 20 μl.The linearly dependent coefficients of bifenthrin,fenpropathrin,permethrin,and deltamethrin were 0.999 6-0.999 8,the linear range was 5-300 μg/L,and the detection limit was 0.03-0.05 μg/L.Standard recovery experiments on Longyun lake water in Xuzhou urban and Lab water were carried out with 2 different concentrations.The recovery rates were 95.4%-107.8%,and the relative standard deviation(RSD) was 2.74%-6.09%(n=6).The detected concentration met the national standards.Conclusion This method is featured in innovative development of pretreatment technology,and usage of green and environment protective organic solvents.The sensitivity is high,and the recovery and reproducibility are good.
Objective To detect trace amounts of bifenthrin,fenpropathrin,permethrin,and deltamethrin in urban sponge water.Methods The extraction was carried out by using solidification of floating organic drop liquid-phase micr-extraction(SFOD-LPME) technique combined with gas chromatography method,and was quickened by the assist of ultraphonic method and surfactants.The results were analyzed with external reference method.Results In this experiment,the ultrasonic time was 1.5 min,the ultrasonic temperature was 20 ℃,the extractant was hexadecane,the dosage was 80 μl,and the optimal dosage of surfactant Tween 20 was 20 μl.The linearly dependent coefficients of bifenthrin,fenpropathrin,permethrin,and deltamethrin were 0.999 6-0.999 8,the linear range was 5-300 μg/L,and the detection limit was 0.03-0.05 μg/L.Standard recovery experiments on Longyun lake water in Xuzhou urban and Lab water were carried out with 2 different concentrations.The recovery rates were 95.4%-107.8%,and the relative standard deviation(RSD) was 2.74%-6.09%(n=6).The detected concentration met the national standards.Conclusion This method is featured in innovative development of pretreatment technology,and usage of green and environment protective organic solvents.The sensitivity is high,and the recovery and reproducibility are good.
引文
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[2] 高清珍,马智玲,周千渝,等.悬浮固化-分散液-液微萃取-气相色谱法测定蔬菜中6种拟除虫菊酯类药物[J].食品工业科技,2014,35(10):53-56.
[3] 李拥军,黄志强,戴华,等.茶叶中多种拟除虫菊酯类农药残留量的气相色谱-质谱测定[J].分析化学研究简报,2002,30(7):865-868.
[4] Du J,Yan H,She D,et al.Simultaneous determination of cypermethrin and permethrin in pear juice by ultrasound-assisted dispersive liquid-liquid microextraction combined with gas chromatography[J].Talanta,2010(82):698-703.
[5] Jeannot MA,Cantwell FF.Solvent microextraction into a single drop[J].Anal Chem,1996,68(13):2236-2240.
[6] Pederson-Bjergaard S,Rasmussen KE.Liquid-Liquid-Liquid microextraction for sample preparation of biological fluids prior to capillary electrophoresis[J].Ana Chem,1999,71(14):2650-2656.
[7] Rezaee M,Assadi Y,Milani Hosseini MR,et al.Determination of organic compounds in water using dispersive liquid-liquid microextraction[J].J Chromatogr A,2006,1116(1-2):1-9.
[8] Zhou QX,Bai HH,Xie GH.Temperature-controlled ionic liquid dispersive liquid phase micro-extraction[J].J Chromatogr A,2008,1177(1):43-49.[8] 王楠,张桂菊,赵莉,等.表面活性剂的性能与应用(Ⅻ)-表面活性剂的分散作用及其应用[J].日用化学工业,2014,44(12):666-675.
[9] 郭亚芸,丁燕,胡效亚,等.表面活性剂辅助-凝固-漂浮分散液液微萃取-高效液相色谱法测定环境水样中酚类化合物[J].分析测试学,2015,34(9):1040-1044.
[10] 杨继生.表面活性剂原理与应用[M].南京:东南大学出版社,2012.
[11] Ahmadvanda M,Sereshtia H,Parasta H.Chemometric-based determination of polycyclic aromatic hydrocarbons in aqueous samples using ultrasound-assisted emulsification microextraction combined to gas chromatography-mass spectrometry[J].J Chromatogr A,2015,1413:117-126.