An amino-functionalized mesoporous silica (KIT-6) as a sorbent for dispersive and ultrasonication-assisted micro solid phase extraction of hippuric acid and methylhippuric acid, two biomarkers for toluene and xylene exposure

The authors described a new application of amino-functionalized KIT-6 for dispersive ultrasonication-assisted micro solid phase extraction of hippuric acid (HA) and methyl hippuric acid (MHA) from human urine and water samples. In the first step, an amino-functionalized mesoporous silica of type KIT-6 was synthesized. It was characterized by field emission scanning electron microscopy, Fourier transform infrared spectrometry, nitrogen adsorption-desorption analysis, thermogravimetry and X-ray diffraction. Following sorption and desorption with 1.0 mL methanol/NH₄OH (1%; v/v), HA and MHA were quantified by HPLC with UV detection. Various important parameters were optimized by Box-Behnken design. Under optimized conditions, The limit of detections (LOD) were calculated by a signal-to-noise ratio of 3, which were 0.5 μg L⁻¹ and 0.2 μg L-1 for HA and MHA, respectively, and the calibration plot is linear in the 1–1000 μg L⁻¹ concentration range. Only small matrix effects were found. The method was successfully implemented for the sensitive determination of HA and MHA in (spiked) human urine samples. .