Multiresidue Pesticide Analysis in Wines by Solid-Phase Extraction and Capillary Gas Chromatography−Mass Spectrometric Detection with Selective Ion Monitoring

Abstract

A method was developed to determine pesticides in wines. The pesticides were extracted from the wine using solid-phase extraction on a polymeric cartridge, and the coextractives were removed with an aminopropyl-MgSO(4) cartridge. Analysis was performed using capillary gas chromatography with electron impact mass spectrometric detection in selective ion monitoring mode (GC-MSD/SIM). Three injections are required to analyze all 153 organohalogen, organonitrogen, organophosphate, and organosulfur pesticides and residues. Pesticides were confirmed by retention times of the target ions and three qualifier-to-target ion ratios. Detection limits for most of the pesticides were less than 0.005 mg/L, and quantitation was determined from approximately 0.01 to 5 mg/L. Spike recoveries were performed by fortifying red and white wines at 0.01 and 0.10 mg/L. At the 0.01 ppm level, the spike recoveries were greater than 70% for 116 and 124 pesticides (out of 153) in red and white wines, respectively, whereas at the higher spike concentration of 0.10 mg/L, the recoveries were greater than 70% for 123 and 128 pesticides in red and white wines, respectively. The recoveries of less than 70% were most likely from pesticide polarity or lability, resulting in the inefficient adsorption of the pesticide to the polymeric sorbent, ineffective elution of the pesticide from the sorbent, or thermal degradation of the pesticide under GC-MSD conditions.

Determination of Pesticide Residues by GC-MS Using Analyte Protectants to Counteract the Matrix Effect

“…Other authors 16 have reported good recovery results in wine samples when calibration standards were prepared with corn oil as an analyte protectant. These facts suggest that the volatility range covered by the mixture of fatty acids gives good analyte protection despite differences in the composition of corn and olive oils.…”

“…Several factors have to be considered in selecting the analyte protectants, such as their volatility and hydrogen-bonding ability. Based on previous studies, 2,3-butanediol, L-gulonic acid γ-lactone 11 and corn oil 16 were selected as protectant agents. Olive oil was also included in the study.…”

Overview of Analytical Techniques for Herbicides in Foods

“…Oxyfluorfen is amenable to GC separation (Wong et al, 2003), and nitrofen, with a similar structure, should have favorable properties for GC. Shen (Shen et al, 2008) extracted DPhE from vegetables sample with acetonitrile, then the extract was cleaned up by Envi-Carb SPE column connected to Alumina Neutral SPE column, determined by gas chromatographynegative chemical ionization mass spectrometry.…”

Non-invasive multiresidue screening methods for the determination of pesticides in heritage collections

“…Methods of pesticide analyses have been largely driven by the food industry [1][2][3]. In their comprehensive paper of 2000, Filion et al [4] screened fruit and vegetable samples for 251 known pesticides by extracting pulp with solvent before clean-up on solid phase extraction cartridges.…”