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Published on: January 28, 2011
High-performance organized media-enhanced spectrofluorimetric determination of pirimiphos-methyl in maize
Milagros Montemurro1, Romina Brasca2, María J Culzoni1
1Laboratorio de Desarrollo Analítico y Quimiometría (LADAQ), Facultad de Bioquímica y Ciencias Biológicas, Universidad Nacional del Litoral, Ciudad Universitaria, Santa Fe 3000, Argentina; Consejo Nacional de Investigaciones Científicas y Técnicas (CONICET), Godoy Cruz 2290, CABA (C1425FQB), Argentina.
Abstract:
A novel method for the determination of pirimiphos-methyl (PMM) in maize grains by fluorescence spectroscopy and three-way calibration was developed. The formation of supramolecular complexes and their effect on the luminescence properties of PMM were studied. A solvent extraction step followed by solid phase extraction for sample clean-up was optimized. A chemometric approach consisting in PARAFAC as second-order data processing tool and piecewise direct standardization (PDS) for reducing the complexity of the calibration process was developed to overcome the matrix effect. This strategy allowed dealing with the matrix effect while reducing the number of samples to be processed and, consequently, the solvent consumption and the total analysis time. Finally, three-way calibration was applied to predict the PMM concentration in unknown samples. The mean recovery was 115% and the limits of detection and quantitation were in the order of the parts per trillion, i.e. 6 and 20 ng g-1, respectively.
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