Determination of 19 multi-residue pesticides in grape wine by gas chromatography-mass spectrometry with micro liquid-liquid extraction and solid phase extraction

A multi-residue method has been developed for the confirmation and quantitation of 19 pesticides in red grape wine. Micro liquid-liquid extraction(LLE) and solid phase extraction(SPE) were compared and gas chromatography-electron ionization mass spectrometry was used for the detection. Recoveries for SPE and micro LLE methods were found in the range of 77.8%-109.1% (137.5% for clofentezine) and 83.3%-116.7% (43% for clofentezine) with RSDs <14%, respectively. For the SPE and micro LLE methods, LODs ranged from 0.001 to 0.01 mg/kg and 0.02 to 0.10 mg/kg, while LOQs ranged from 0.005 to 0.05 mg/kg and 0.06 to 0.30 mg/kg, respectively, depending on the sensitivity of each compound. All of the targets had matrix enhancement effect, which could be reduced by using matrix-matched calibration solutions.