HPLC Determination of Buprofezin and Pyridaben in Water Samples with Separation by Dispersion Liquid-Liquid Microextraction
摘 要
取水样置于离心管中,与含有三氯甲烷(萃取溶剂)的乙腈(分散剂)混合溶液充分混匀,静置5 min,使水样中的扑虱灵和哒螨灵迅速富集于三氯甲烷液滴中,离心5 min,下层三氯甲烷相经减压蒸干后,加入乙腈-水(75+25)混合溶液50 μL溶解残渣,分取20 μL溶液供高效液相色谱法分析。用Symmetry C18色谱柱作固定相,流动相为乙腈-水(75+25)混合溶液,检测波长为238 nm。扑虱灵和哒螨灵的线性范围分别为2.0~100 μg·L-1和1.0~100 μg·L-1。回收率分别在81.2%~99.2%和87.3%~100.7%之间,相对标准偏差(n=5)分别在1.7%~8.3%及0.6%~9.1%之间。
Abstract
Two insecticides, buprofezin (BPFZ) and pyridaben (PRDB) were separated from water sample by mixing thoroughly with a mixture containing CH3CN and CHCl3 and standing for 5 min in a centrifuge tube. After centrifuging for 5 min, the solvent CHCl3 was removed by evaporation under reduced pressure and the residue was taken up with 50 μL of mixed solvent of CH3CN and water (75+25), from which an aliquot of 20 μL was taken for HPLC analysis. Symmetry C18 column was used as stantionary phase and mixture of CH3CN and water (75+25) as mobile phase. UV detection at 238 nm was adopted in the determination. Linearity ranges were found between 2.0-100 μg·L-1 (for BPFZ) and 1.0-100 μg·L-1 (for PRDB). Values of recovery and RSD′s (n=5) found were in the ranges of 81.2%-99.2%, 87.3%-100.7%, and 1.7%-8.3%, 0.6%-9.1% respectively.
中图分类号 O657.7
所属栏目
基金项目 国家自然科学基金项目(20977025);河南省教育厅自然科学基金项目(2009A150016);河南师范大学青年科学基金(2008qk12)
收稿日期 2010/11/20
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备注叶存玲(1973-),女,河南洛阳人,副教授,主要从事分析化学方面的教学和科研工作。
引用该论文: YE Cun-ling,LIU Qing-ling,XIE Guo-hong,WANG Zhi-ke. HPLC Determination of Buprofezin and Pyridaben in Water Samples with Separation by Dispersion Liquid-Liquid Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(12): 1391~1394
叶存玲,刘清玲,谢国红,王治科. 分散液相微萃取-高效液相色谱法测定水样中扑虱灵和哒螨灵[J]. 理化检验-化学分册, 2011, 47(12): 1391~1394
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【3】田孟魁,冯喜兰.固相微萃取-气相色谱法测定橙汁中残留有机氯杀虫剂[J].理化检验-化学分册, 2008,44(9):833-836,839.
【4】DADFARNIA S, SHABANI A M H. Recent development in liquid phase microextraction for determination of trace level concentration of metals-A review [J]. Anal Chim Acta, 2010,658(2):107-119.
【5】BASHEER C, ALNEDHARY A A, MADHAVA R B S, et al. Ionic liquid supported three-phase liquid-liquid-liquid microextraction as a sample preparation technique for aliphatic and aromatic hydrocarbons prior to gas chromatography-mass spectrometry[J]. J Chromatogr A, 2008,1210(1):19-24.
【6】JEANNOT M A, PRZYJAZNY A, KOKOSA J M. Single drop microextraction-development, applications and future trends[J]. J Chromatogr A, 2010,1217(16):2326-2336.
【7】AMVRAZI E G, TSIROPOULOS N G. Chemometric study and optimization of extraction parameters in single-drop microextraction for the determination of multiclass pesticide residues in grapes and apples by gas chromatography mass spectrometry[J]. J Chromatogr A, 2009,1216(45):7630-7638.
【8】DAI L, CHENG J, MATSADIQ G, et al. Dispersive liquid-liquid microextraction based on the solidification of floating organic droplet for the determination of polychlorinated biphenyls in aqueous samples[J]. Anal Chim Acta, 2010,674(2):201-205.
【9】藏晓欢,吴秋华,张美月,等.分散液相微萃取技术研究进展[J].分析化学, 2009,37(2):161-168.
【10】REZAEE M, YAMINI Y, FARAJI M. Evolution of dispersive liquid-liquid microextraction method[J]. J Chromatogr A, 2010,1217(16):2342-2357.
【11】李鱼,刘建林,王晓丽,等.分散液-液微萃取/高效液相色谱法测定水样中的痕量双酚A[J].高等学校化学学报, 2008,29(11):2142-2148.
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