Determination of Residues of Carbofuran and 3-Hydroxycarbofuran in Bee Products by Liquid Chromatography Tandem Mass Spectrometry with QuEChERS

A method for determination of residues of carbofuran and 3-hydroxycarbofuran in bee products (honey, propolis and royal jelly) was proposed by QuEChERS pretreatment combined with liquid chromatography tandem mass spectrometry (LC-MS/MS). The bee product sample was extracted with acetonitrile, dehydrated by anhydrous magnesium sulfate, and purified with the mixed agent of anhydrous magnesium sulfate, PSA and C₁₈. Accucore aQ C₁₈ column (150 mm×2.1 mm, 2.6 μm) was used for the separation, and the mixtures of methanol and 0.1% (volume fraction) formic acid solution containing 5 mmol·L^-1 ammonium formate at different volume ratios were used as the mobile phase for gradient elution. Multiple reaction monitoring (MRM) mode was adopted in MS detection, with external standard method for quantification. As shown by the results, linear relationships between values of the corresponding peak area and mass concentration of carbofuran and 3-hydroxycarbofuran were found in the range of 0.002-0.100 mg·L^-1, with lower limits of determination (10S/N) of carbofuran and 3-hydroxycarbofuran in honey and royal jelly of 0.01 mg·kg^-1, and those in propolis of 0.05 mg·kg^-1. Test for recovery was made by the standard addition method, giving the results in the range of 84.5%-108%, with RSDs (n=6) of the determined values less than 7.0%.