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胶束毛细管电泳分析杀虫剂幻灯片.pdf

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Journal of Chromatography A, 1153 (2007) 104–113 On-line preconcentration strategies for analyzing pesticides in fruits and vegetables by micellar electrokinetic chromatography ´ ´ ∗ Ana Juan-Garcıa, Guillermina Font, Yolanda Pico Laboratori de Bromatologia i Toxicologia, Facultat de Farm`acia, Universitat de Val`encia, Av. Vicent Andr´es Estell´es s/n, 46100 Burjassot, Val`encia, Spain Available online 4 February 2007 Abstract Five pesticides (fludioxonil, procymidone, pyriproxyfen, dinoseb and carbendazim) were separated in reversed migration micellar electrokinetic chromatography (RM-MEKC) using 20 mmol l−1 phosphate buffer at pH 2.3, containing 25 mmol l−1 sodium dodecylsulfate and 10% methanol. Three on-line concentration strategies, sweeping (SW), normal stacking with reversed migration and a water plug (SRW) and stacking with reverse migration and removal of sample matrix using polarity switching (SRMM), were compared. About 10-, 30- and 50-fold increases in detection sensitivity, compared with standard hydrodynamic injection (5 s at 0.5 psi), were observed with SW, SRW and SRMM, respectively. Limits of detection (LODs) ranged from 0.002 to 0.03 g ml−1 using only the on-line preconcentration procedures without any off-line concentration of the extract. A solid-phase extraction (SPE) procedure, for previous isolation and concentration of the analytes, was used in combination with any of the proposed on-line preconcentration strategies, which achieves the determination of pesticides at limits of quantification (LOQs) lower than 0.01 mg kg−1. The recoveries obtained by

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