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Rapid determination of fosetyl-aluminum residues in lettuce by liquid chromatography/electrospray tandem mass spectrometry
Authors:Hernández Félix  Sancho Juan V  Pozo Oscar J  Villaplana Carme  Ibáñez María  Grimalt Susana
Affiliation:University Jaume I, Experimental Sciences Department, Analytical Chemistry, E-12071, Castellón, Spain. hernandf@exp.uji.es
Abstract:
This paper describes a new method for the sensitive and selective determination of fosetyl-aluminum (Al) residues in vegetable samples. The method involves extraction with water by using a high-speed blender and subsequent injection of the 5-fold diluted extract into the liquid chromatograph. Fosetyl-Al is determined by liquid chromatography with electrospray tandem mass spectrometry after the addition of tetrabutylammonium acetate as the ion-pairing reagent. The method has been used to assay lettuce samples spiked at 2 and 0.2 mg/kg. Recoveries were satisfactory, with mean values of 98 and 106%, respectively, and relative standard deviations were < 10%. The limit of quantitation was 0.2 mg/kg, and the limit of detection was as low as 0.05 mg/kg. Matrix-matched calibration was used for quantitation, and the addition of an internal standard improved repeatability. The developed method allows the accurate and rapid determination of low levels of fosetyl-Al residues in lettuce with very little sample handling and good sensitivity; it was shown to be robust by the analysis of almost 100 samples.
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