Ana Aguilera, Antonio Valverde, Antonio Valverde-Monterreal, Luis Garcia-Fuentes, Mourad Boulaid
Journal of environmental science and health. Part. B, Pesticides, food contaminants, and agricultural wastes 2014Derivatization of cyprodinil with different reagents and solvents has been evaluated to improve the GC/MS characterization of this fungicide. After assessing some preliminary acylation and silylation reactions, derivatization with anhydrous heptafluorobutyric anhydride (HFBA) was selected as the best derivatization option for cyprodinil. The HFBA-cyprodinil derivative was clearly identified and characterized by GC/MS (ion-trap). The spectrum of the HFBA derivative of cyprodinil was characterized by the base peak, 252 m/z ion, and two other ions with relative abundances of 5% (224 m/z ion) and 4% (420 m/z molecular ion). Conversion rates in the range of 83-92% were obtained when 0.1-1 μg cyprodinil were derivatized in vial without solvent at 25ºC temperature for 120 min, with 5 μL HFBA and 5 μL pyridine. Simultaneous extraction-derivatization of cyprodinil in supercritical carbon dioxide was only achieved when no modifier was present, but conversion/recovery rates obtained in the replicate experiments carried out with 15 mL supercritical carbon dioxide at 50°C and 200 atm (n = 5), 300 atm (n = 7), and 400 atm (n = 5) were no reproducible (RSD > 50%) and ranged between 10% and 45% (related to the signal obtained for derivatization in vial).
Ana Aguilera, Antonio Valverde, Antonio Valverde-Monterreal, Luis Garcia-Fuentes, Mourad Boulaid. Assessing solvent derivatization and carbon dioxide supercritical fluid simultaneous extraction/derivatization of cyprodinil. Journal of environmental science and health. Part. B, Pesticides, food contaminants, and agricultural wastes. 2014;49(8):541-9
PMID: 24901957
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