Liquid chromatographic determination of flumetsulam in soybeans

Michael Moawad, Cheang Khoo

    Research output: Contribution to journalArticle

    3 Citations (Scopus)

    Abstract

    A liquid chromatography (LC) method with UV detection is reported for the determination of the sulfonamide herbicide flumetsulam in soybeans. The ground soybean sample was partitioned between methanol and hexane. The hexane removed the lipids, and the methanol layer containing the analyte was further partitioned between dichloromethane and aqueous phosphate buffer at pH 7.0. The aqueous layer, containing the analyte, was acidified to pH 2.2 and partitioned with fresh dichloromethane. The dichloromethane layer containing the analyte was evaporated, and the residue was dissolved in the LC mobile phase for analysis. A polar embedded C18 column was used with a mobile phase of pH 2.2 aqueous phosphate buffer-acetonitrile (68 + 32), run isocratically with detection at 225 nm. The average recovery was 82% with a relative standard deviation (RSD) of 10%. A coefficient of determination of [R.sup.2] = 0.9992 was achieved for the analyte calibration curve, from 0.005 to 1 lag/mL. The limit of detection, determined from 3 times the standard deviation of 7 replicate extractions of the lowest fortification level (0.01 Vg/g), was 0.005 Pg/g with an RSD of 22%. LC/electrospray ionization/mass spectrometry in the positive-ion mode was used for identity confirmation of flumetsulam in the fortified soybean extract. The ions at m/z 326, 348, and 129 were observed.
    Original languageEnglish
    Number of pages6
    JournalJournal of AOAC International
    Publication statusPublished - 2005

    Keywords

    • flumetsulam
    • herbicides
    • liquid chromatography
    • soybean

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