Magnetic MCM-41 functionalized with ureathiosemicarbazone monohydrate as the sorbent for magnetic solid-phase extraction of triazole fungicides from fruit samples followed by measuring using high performance liquid chromatography

In this study, a novel sorbent called MCM-41-ureathiosemicarbazone monohydrate@Fe3O4 was developed for magnetic solid-phase extraction (MSPE) to extract two selected triazole fungicides including propiconazole and tebuconazole in apple, strawberry, orange, carrot, spinach and various wastewater samples. The sorbent was synthesized using MCM-41 and functionalized with ureathiosemicarbazone monohydrate (UTM). The synthesized sorbent was characterized by various characterization methods to approve the successful synthesis of the sorbent. The separated analytes were measured using high-performance liquid chromatography coupled with ultraviolet detection (HPLC-UV). After fine-tuning, the technique showed a linear range of 1.00-200.00 mu g L- 1 for the desired compounds, with correlation coefficients (r2) higher than 0.9972. The limits of detection (LODs) were found to be between 0.29 and 0.31 mu g L- 1. The limits of quantification (LOQs) were also between 0.96 and 1.03 mu g L- 1. The inter-day and intra-day precision, indicated by relative standard deviations (%RSDs), ranged from 2.2 to 5.9 %. The batch-to-batch RSDs were also in the range of 3.2-3.5 % (for the concentration of 50 mu g L- 1). The enrichment factor (EF) values for the tested substances varied from 25 to 27. The absolute recoveries (ARs%) were also 27 % and 25 %. Recovery rates indicated the capability of the proposed method for pesticide analysis in selected real samples. The obtained relative recoveries were between 90 and 101 %. Moreover, the calculated spiking recoveries were in the range of 90-110 %. The results showed good accuracy and precision of the developed method for the determination of trace amounts of target analytes. In addition, the greenness and whiteness of the method (sustainability assessment) were evaluated using the qualitative green assessment tool including AGREE, BAGI and the white analytical chemistry assessment tool (RGB12). The high BAGI (70) and RGB 12 (89.5) scores confirmed the method's strong applicability, cost-effectiveness, and sustainability.