MSPD METHOD FOR THE DETERMINATION OF CLOFENTEZINE, FLUMETRALIN, AND KRESOXIM-METHYL RESIDUES IN FRESH AND DEHYDRATED FORMS OF PLANTAGO MAJOR MEDICINAL PLANT BY HPLC/UV-DAD

Abstract

A method was developed using matrix solid-phase dispersion (MSPD), together with liquid chromatography with ultraviolet diode array detector for determination of clofentezine, flumetralin, and kresoxim-methyl in fresh and dehydrated Plantago major medicinal plant material. Parameters evaluated included the type of sorbent (C₁₈-bonded silica, neutral alumina, silica gel, Florisil, and MIL-53) using dichloromethane as the eluting solvent. The best results were obtained using 0.5 g of plant material, 0.5 g of silica gel as sorbent, and dichloromethane (20 mL). The method was validated using plant samples spiked with pesticides at three concentration levels (0.5, 1.0, and 2.0 µg/g). Average recoveries (using four replicates) ranged from 62.2% to 110%, with relative standard deviations between 5.4% and 18.5%. Detection and quantification limits were in the ranges 0.05–0.07 µg/g and 0.15–0.25 µg/g, respectively.

Keywords:

• LC
• matrix solid-phase dispersion
• medicinal plant
• metal organic framework
• pesticides
• Plantago major

ACKNOWLEDGMENT

The authors wish to thank MCT/CNPq (process number 620247/2008-8) for financial support of this study. E. S. Silvia dos Santos also thanks CAPES for provision of a research fellowship.

Notes

Note. Plantago major sample fortified at 1.0 µg/g.

^a n = 3.

^a n = 4.