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Factors affecting the extraction, hydrolysis and derivatization steps for the quantitation of total residues of amitraz in honey by gas chromatography with electron capture detection

Jiménez, J., Nozal, M., Bernal, J., Santos, M., Mayorga, A.
Analytical and bioanalytical chemistry 2002 v.374 no.2 pp. 300-304
derivatization, aqueous solutions, food contamination, liquid-liquid extraction, ambient temperature, pesticide residues, pH, solvents, hydrolysis, hexane, gas chromatography, solid phase extraction, honey, amitraz
A study about the most adequate conditions for the determination of the amitraz total residues in honey by gas chromatography is presented. Solvent and solid phase extraction procedures as well as the influence of several parameters on the extraction, hydrolysis and derivatization steps are considered. Solid phase extraction on ODS cartridges was found to be not reliable for the determination of total residues, because recovery for 2,4-dimethylaniline (DMA) was poor. Liquid–liquid extraction with hexane was accomplished in a single step and was more reproducible. The pH of the aqueous solution had to be set at pH 11 to achieve extraction of DMA. The derivatization of DMA with heptafluorobutyric anhydride (HFBA) was practically instantaneous at room temperature.