Development of an analytical method for determination of total ethofumesate residues in foods by gas chromatography-tandem mass spectrometry
2020
Saito-Shida, Shizuka | Kashiwabara, Nao | Shiono, Kouji | Nemoto, Satoru | Akiyama, Hiroshi
Analytical method was developed for determining the total residue of ethofumesate (ET) herbicide using GC–MS/MS. The ET residues were analyzed as a sum of ET, 2-keto-ethofumesate (KET), and open-ring-2-keto-ethofumesate (OKET) and its conjugate. The extracted samples were partitioned with hexane and NaOH solution. For ET analysis, the hexane layer was cleaned up by a silica gel cartridge prior to GC–MS/MS analysis. For the analyses of the metabolites, the aqueous layer was heated with HCl to hydrolyze the conjugates, thereafter, heated in acetic anhydride to convert OKET to KET, and cleaned up by a silica gel cartridge prior to GC–MS/MS analysis. The method was validated for ET, KET, and OKET in garlic, onion, and sugar beet at 0.3 and 0.01 mg/kg. The recoveries were 94–113%, with relative standard deviations of <6%. The limits of detection were 0.0005 mg/kg for all analytes. The proposed method is suitable for regulatory analysis.
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