A MOF with high specific surface area for rapid separation and determination of β-adrenergic receptor blockers in pork by open-tubular capillary electrochromatography

Abstract

In this work, a novel Ti-based MOF (NH2-MIL-125) bonded open-tubular (OT) column was firstly prepared via one-step in-situ growth method for capillary electrochromatography (CEC). The stationary phase was characterized by Fourier transform-infrared spectroscopy, scanning electron microscopy, X-ray diffraction spectroscopy, and nitrogen adsorption-desorption measurements. The results showed that the stationary phase exhibited a large specific surface area (1247.57 m²/g) with microporous and mesoporous structure and no obvious changes in the morphology/size inside and outside the column. Baseline separation of three β-adrenergic receptor blockers (Prop, Sot, and Lab), three β-adrenergic receptor agonists, and four sulfonamide antibiotics were obtained under the optimized CEC conditions with the shortest analysis time of 2.52 min and a maximum resolution of 11.52. The separation mechanisms were mainly attributed to polarity and electrophoretic mobility of the analytes, as well as π-π interactions and hydrogen bonding interaction between the stationary phase and the analytes. A quantitative detection method of three β-adrenergic receptor blockers in pork samples was established using the NH2-MIL-125 bonded OT column. Good linearity (R² > 0.999) was obtained over the concentration range of 0.01-1.00 mg/mL with limits of detection of 0.0044-0.0084 mg/mL and recoveries of 90.27-106.74%. Thus, the developed method was simple, rapid and high efficiency, and could be applied for the simultaneous separation and detection of the three β-adrenergic receptor blockers in real samples.