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Sensitive determination of urinary muconic acid using magnetic dispersive-solid-phase extraction by magnetic amino-functionalised UiO-66

ABSTRACT In this study, a magnetic-dispersive solid-phase extraction (DSPE) was developed for the extraction and desorption of muconic acid from real urine sample. For this purpose, Fe3O4-SiO2-NH2@ UiO-66 was used as a Metal-Organic Framework (MOF) in the DSPE for extraction of the analyte of interest followed by High-Performance Liquid Chromatography (HPLC) analysis. The synthesised magnetic-MOF was characterised by XRD, VSM, FT-IR, and FE-SEM techniques. The experimental parameters influencing the magnetic-DSPE procedure, such as solution pH, initial sample volume, extraction and desorption time, type and volume of elution solution, and sorbent amount were examined. Under the optimal conditions, the UiO-magnetic DSPE-HPLC procedure provided a good limit of detection (0.001 µg mL−1), the limit of quantification (0.003 µg mL−1), wide linear dynamic range (0.003–25 µg mL−1) and high correlation coefficient (r2: 0.997). Also, the Fe3O4- SiO2- NH2@ UiO-66 exhibited an acceptable accuracy (2.0–4.0%), reproducibility (3.7–6.1%), and per cent recovery (96–98%) for the extraction and desorption of the desired analyte. It can be concluded that the proposed method was efficient for the extraction and analysis of muconic acid from real urine samples. Therefore, the Fe3O4- SiO2- NH2@ UiO-66 – DSPE-HPLC method can be used as a simple, fast, sensitive, reusable, and user-friendly extraction technique to determine trace levels of urinary muconic acid.