LC/ESI–MS/MS method for the identification and quantification of spinosad residues in olive oils

Abstract

This paper reports the use of liquid chromatography/electrospray ionisation tandem mass spectrometry (LC/ESI-MS/MS) method for the identification and quantification of residues of the natural insect control agent Spinosad in olive oils. The method determines the active ingredients Spinosyns A and D and two minor metabolites Spinosyns B and K without laborious sample treatment. All four analytes are determined simultaneously in a single injection using positive electrospray ionisation LC–MS with multiple reaction monitoring (MRM). For the quantitative analysis of samples an external calibration curve was built. The calibration curves for each analyte were linear in the concentration range 20–500 ng/mL with a correlation coefficient ranging between 0.995 and 0.999. Results from spike and recovery experiments at levels of 100 and 200 ng/mL gave mean recoveries ranging from 87–116% with satisfactory precision (relative standard deviation (RSD) from 1–8%). The excellent selectivity and sensitivity allows quantification and identification of low levels of Spinosad in olive oils (limits of quantification (LOQs) 0.004–0.073).