Pest Management Science · 2004 · 40 citations · 15 references
PharmacyPharmaceutical AnalysisAnalytical ChemistryChromatographic AnalysisSeparation ScienceAnalytical ChromatographyChromatographyExtraction TechniquesLiquid ChromatographyLiquid-liquid ExtractionSolvent ExtractionAnalytical Liquid ChromatographyHigh-performance Liquid ChromatographyHigh-performance Liquid Chromatography ColumnsHigh-performance Liquid Chromatography Method DevelopmentLiquid - Liquid Phase SeparationRecovery Of Pharmaceutical Compounds
A practical method for analysis of residues of imidacloprid in baked tobacco leaves has been developed using HPLC with liquid-liquid partition clean-up. Imidacloprid was extracted with ethyl acetate under ultrasound, and cleaned up by liquid-liquid partition with 50 g litre(-1) aqueous sodium chloride followed by dichloromethane. The water-soluble and fat-soluble components in tobacco, which interfere with imidacloprid in HPLC, were removed. The separation was performed on a Supelco LC-18 column (250 mm x 4.6 mm ID) with a mobile phase of acetonitrile + 5 mM ammonium acetate (20 + 80 by volume) at a flow-rate of 1 ml min(-1). The baseline separation between imidacloprid and the tobacco blank was achieved within 10 min. With a detection wavelength at 270 nm, the limit of quantitation was 0.04 mg kg(-1). The recovery ranged from 89.8 to 95.4% and the RSDs were less than 2.3%. The proposed method was successfully employed for the determination of imidacloprid residues in 300 samples of flue-cured tobacco leaves.
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Hirotaka Obana, Msahiro Okihashi, Kazuhiko Akutsu et al. · Journal of Agricultural and Food Chemistry · 2002 · 202 citations
Hirotaka Obana, Masahiro Okihashi, Kazuhiko Akutsu et al. · Journal of Agricultural and Food Chemistry · 2003 · 189 citations