Simultaneous Determination of 69 Pesticide Residues in Coffee by Gas Chromatography–Mass Spectrometry

Abstract

A method using gel permeation chromatography (GPC) combined with solid-phase extraction (SPE) cleanup followed by gas chromatography–mass spectrometry (GC-MS) has been established for quantitative determination of 69 pesticide residues in coffee. Based on an appraisal of the characteristics of GC-MS, validation experiments were conducted for 69 pesticides. In the method, 2.0 g samples were mixed with 5 ml water and 1 g sodium chloride and extracted with 5 ml of ethyl acetate by blender homogenization, centrifugation, and filtration. Evaporation was conducted and the sample was injected into a 250 mm × 10 mm S-X3 GPC column, with ethyl acetate–n-hexane (1:2 v/v) as the mobile phase at a flow rate of 3 ml/min. The 4–15 min fraction was collected for the SPE cleanup, which was Envi-Carb SPE cartridge coupled with NH₂-LC SPE cartridge with acetone–ethyl acetate (2:5 v/v) as the eluted solvent. The eluents were collected and then evaporated to dryness, which was redissolved in 0.5 ml ethyl acetate for GC-MS analysis. For the 69 pesticides determined by GC-MS, the portions collected from GPC were concentrated to 0.5 ml and exchanged with 5 ml n-hexane. In the linear range of each pesticide, the correlation coefficient was R ² ≥ 0.99. At the low, medium, and high fortification levels of 0.05–1.0 mg/kg, recoveries fell within 60–120%. The relative standard deviation was between 1.3% and 22.3% for all 69 pesticides. The limits of detection for the method were 10 μg/kg to 150 μg/kg, depending on each pesticide.