Quantification of neonicotinoid insecticide residues in soils from cocoa plantations using a QuEChERS extraction procedure and LC-MS/MS

Abstract

The use of neonicotinoids as an insecticide group in Ghana has been quite significant particularly in cocoa production. The high usage has been mainly as a result of a government policy of free insecticide spraying on cocoa farms, in an effort to curb declining yields caused by pests and diseases and to prevent the use of unapproved or banned insecticides on cocoa farms. However the scale of cocoa farming, the frequency and intensity of usage coupled with the mode of application may result in large physical volumes of insecticides in the environment. This makes the knowledge of the concentration and fate of neonicotinoids in the environment extremely important. The present study was aimed at assessing the levels of five major neonicotinoids in soils from cocoa farmlands in Ghana. Extraction and cleanup of analytes were performed by use of a method based on the original QuEChERS procedure after optimizing salts, sorbents and instrumental conditions. Analyte extraction with NaCl and MgSO4 in acidified acetonitrile followed by cleanup with primary secondary amine (PSA) presented the optimum conditions for extraction. Quantification was performed using liquid chromatography-tandem mass spectrometry (LC-MS/MS) with electrospray ionization (ESI). Validation of the procedure showed average recoveries ranging from 72.0 to 104.8% for all analytes at all fortification levels with relative standard deviation (RSD)≤15.0. Limits of quantitation were<10μgkg−1 for all neonicotinoids studied. The results obtained from the analysis of 52 samples from cocoa farms revealed imidacloprid as the predominant neonicotinoid with concentrations ranging from 4.3 to 251.4μgkg−1 in>50% of samples analyzed.