A low-cost biosorbent-based coating for the highly sensitive determination of organochlorine pesticides by solid-phase microextraction and gas chromatography-electron capture detection

Abstract

In this study, an environmentally friendly and low-cost biosorbent coating was evaluated, for the first time, as the extraction phase for solid-phase microextraction (SPME) supported on a nitinol alloy. The characterization of the new fiber was performed by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The applicability of the biosorbent-based fiber in the determination of δ-hexachlorocyclohexane, aldrin, heptachlor epoxide, α-endosulfan, endrin and 4,4′-DDD in water samples was verified, with separation/detection by gas chromatography coupled to electron capture detection (GC-ECD). The influencing parameters (temperature, extraction time and ionic strength) were optimized simultaneously using a central composite design. The optimum conditions were: extraction time of 80min at 80°C and sodium chloride concentration of 15% (w/v). Satisfactory analytical performance was achieved with limits of detection (LOD) between 0.19 and 0.71ngL−1 and limits of quantification (LOQ) between 0.65 and 2.38ngL−1. The relative recoveries for the analytes were determined using river and lake water samples spiked at different concentrations and ranged from 60% for α-endosulfan to 113% for δ-hexachlorocyclohexane, with relative standard deviations (RSD) lower than 21%. The fiber-to-fiber reproducibility (n=3) was also evaluated and the RSD was lower than 14%. The extraction efficiency obtained for the proposed biosorbent coating was compared to a commercially available DVB/Car/PDMS coating. The proposed fiber provided very promising results, including LODs at the level of parts per trillion and highly satisfactory thermal and mechanical stability.