Matrix solid-phase dispersion extraction and determination by high-performance liquid chromatography with fluorescence detection of residues of glyphosate and aminomethylphosphonic acid in tomato fruit

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• 作者：M.P. Garcí ; a de Llasera ; L. Gó ; mez-Almaraz ; L.E. Vera-Avila ; A. Peñ ; a-Alvarez
• 关键词：Matrix solid-phase dispersion ; Anion exchange cleanup ; FMOC derivatization ; HPLC ; Glyphosate ; AMPA ; Residues ; Tomato fruit ; Herbicides
• 刊名：Journal of Chromatography A
• 出版年：2005
• 出版时间：4 November 2005
• 年：2005
• 卷：1093
• 期：1-2
• 页码：139-146
• 全文大小：338 K

文摘

A method based on matrix solid-phase dispersion (MSPD) is described for the quantitative extraction of glyphosate and its major metabolite aminomethylphosphonic acid (AMPA) from tomato fruit. After application of 120 μL of HNO₃ 1 M to the sample, the dispersion column was packed with 0.5 g of sample blended into 1 g of NH₂-silica. Two aqueous fractions were obtained. First, AMPA was eluted from the column using deionized water (F1), and then a NaH₂PO₄ 0.005 M solution was used for the elution of glyphosate (F2). Cleanup of F1 and F2 was made by ion exchange chromatography on a SAX anion exchange silica. Determination was done by HPLC with fluorescence detection after precolumn derivatization with 9-fluorenylmethylchloroformate (FMOC-Cl). Mean recoveries calculated at fortification levels of 0.5 μg/g for glyphosate and 0.4 μg/g for AMPA were 87 % and 78 % , respectively. The relative standard deviations (n = 7) for the total procedure were 10 % and 16 % . Detection limits were 0.05 μg/g for glyphosate and 0.03 μg/g for AMPA.