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Simple analytical method for determination of pesticide residues in human serum by liquid chromatography tandem mass spectrometry
Authors:Manel Araoud  Wahiba Douki  Mohamed Fadhel Najjar  Abderraouf Kenani
Affiliation:1. Laboratory of Biochemistry, Faculty of Medicine of Monastir , Tunisia;2. Laboratory of Biochemistry-Toxicology , University Hospital Fattouma Bourguiba Monastir , Tunisia;3. Laboratory of Biochemistry-Toxicology , University Hospital Fattouma Bourguiba Monastir , Tunisia;4. Laboratory of Biochemistry, Faculty of Medicine of Monastir , Tunisia
Abstract:The aim of this study was to develop an analytical method for the determination of residues of organophosphorus and carbamate pesticides which are widely used in Tunisia. This method involves a liquid-liquid extraction procedure followed by liquid chromatography tandem mass spectrometry (LC/MS/MS) for the identification and quantification of compounds. Ionization of molecules was performed by the electrospray mode. Multiple reactions monitoring (MRM) was the acquisition mode used for the monitoring of two MS/MS transitions for each compound. The average recoveries obtained, at three different fortification levels, ranged between 65% and 106% for most of the pesticides studied, except for methamidophos (lower than 25%).The linearity of the method was in the range of 5 to 50 μ g/L with a correlation coefficient from 0.995 to 0.999, depending on the analyte. The estimated limit of detection and limit of quantification were 2 μ g/L and 5 μ g/L, respectively. The precision of the analytical procedure was satisfactory and the coefficients of variation, evaluated at three concentration levels were lower than 15% for most pesticides studied. The application of the method was investigated in a population of agricultural workers chronically exposed to various pesticides some of which, such as carbofuran, carbendazim, methomyl and pirimicarb, were detected in some serum samples.
Keywords:Agricultural workers  analytical method  human serum  liquid chromatography tandem mass spectrometry  pesticide residues  validation  LC/MS/MS
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