Determination of endosulfan isomers and their metabolites in tap water and commercial samples using microextraction by packed sorbent and GC–MS

Abstract

A simple, rapid, accurate and sensitive method using microextraction by packed sorbent (MEPS) followed by GC-MS has been pursued for the determination of organochlorine insecticide endosulfan isomers (α and β) and their metabolites (ether, lactone and sulfate). MEPS is a miniaturised version of SPE employing C18 packing material. It is very efficient technique as it employs as low as 10 μL of sample volume. The distinct feature of MEPS is the magnitude of the elution volume that could be directly injected to GC system. Various parameters such as extraction cycles, washing solvent, elution solvent, elution volume and pH, which influenced the MEPS performance, were tested and optimised. The calibration curves were obtained in the concentration range 1-500 ng/mL. The results showed a close correlation coefficient (R(2) > 0.991) for all analytes in the calibration range studied. The LOD and LOQ obtained for GC-MS under selected ion monitoring acquisition are between 0.0038-0.01 and 0.0125-0.033 ng/mL, respectively. The developed method is applicable for the quantification of these compounds in tap water and commercial samples. This method has been shown to be selective as no interferences from endogenous substances were detected by analysis. This method not only decreases sample preparation time but is cheaper, eco-friendly and easier to perform compared to traditional techniques.