An analytic procedure was developed for the determination of the fungicides ametoctradin, boscalid, cyazofamid, dimethomorph, fenhexamid, kresoxim-methyl, mepanipyrim, metrafenone, and pyraclostrobin in grape and wine. A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure was used for the extraction. Analysis of the extract was performed by LC/triple quadrupole-MS/MS. A Poroshell 120 EC-C18 column was used with a programmed gradient mobile phase consisting of (A) acetonitrile containing 0.1% formic acid and (B) water containing 0.1% formic acid and 2 mM ammonium formate. The acceptance criteria for the method were those proposed in the SANCO guide. The method was linear for the range of concentration studied (5-100 μg/L), and R2 values were higher than 0.998 and RSD values below 18%. Recovery was over 73.2% in grape and 76.7% in wines, and there was no case of more than 100% recovery. The recovery RSDs in reproducibility conditions were below 17.13% in grape and 15.6% in wines.
An analytical procedure was developed for the determination of some natural pesticides (piperonyl butoxide, nicotine, rotenone, spinosad, and abamectin B1a) in fruit matrixes. The quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was used for extraction. Analysis of the extract was performed by LC-electrospray ionization (ESI)-MS/MS. The ions prominent in the ESI spectra were [M+Na]+ for abamectin B1a, [M+NH4]+ for piperonyl butoxide, and [M+H]+ for the rest of the compounds. A Zorbax SB-C18 column was used with a programmed gradient mobile phase consisting of (A) water containing 0.1% formic acid and 5 mM ammonium formate, and (B) acetonitrile containing 2 mM sodium acetate. The method was linear within the investigated concentration range, displaying a calibration curve correlation factor of 0.99. The CVs obtained were below 20%, and recoveries were in the 70-110% range.
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