Magnetic layered double hydroxides for the sensitive dispersive solid phase microextraction of hippuric acid in urine samples prior to HPLC-UV analysis

Abstract

The core- shell structural layered double hydroxide (Fe3O4-SiO2-EN@Zn-Al-LDH) was successfully synthesized and applied as a solid sorbent in the magnetic dispersive micro solid-phase-extraction (M-DµSPE) method. It was combined with high-performance liquid chromatography for the trace analysis of hippuric acid (HA) from urine samples. The obtained magnetic layered double hydroxides (LDHs) were characterized by XRD, FT-IR, VSM, FE-SEM, and BET techniques. The characterization analysis indicated that Fe3O4- SiO2- EN@ Zn-Al-LDH has a sufficient surface area and good saturation magnetism. The affecting variables on the extraction of HA by the proposed method were optimized. Excellent adsorption capacity (127.8 mg g−1), wide linearity dynamic range (0.015–500 µg mL−1), and satisfactory limits of detection and quantification (0.055 and 0.014 µg mL−1, respectively) could be obtained under optimum conditions. The good repeatability and low relative standard deviation (7.2 %), low carry-over (2.7%), good matrix effect (93.6%), high reusability (up to 19 times), and an acceptable percent recovery value (97.2%) proved the selectivity and applicability of the proposed method for the extraction of the trace levels of HA in real urine samples.