Synthesis of azo-linked covalent organic polymers for pipette tip solid-phase extraction of sedative residues from...

Azo-linked covalent organic polymers (ACOPs) were synthesized by a simple azo reaction, with 2,2'-bis(trifluoromethyl)benzidine and 1,3,5-trihydroxybenzene as the monomers. The preparation process was mild, green, and environmental-friendly, avoiding the use of high temperature, metal catalysis, and harmful organic reagent. The obtained ACOPs were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, powder X-ray diffraction, and Brunauer-Emmett-Teller. With the prepared ACOPs as adsorbent, a method of pipette tip solid-phase extraction-liquid chromatography-tandem mass spectrometry detection (PTSPE-LC-MS/MS) was proposed for the analysis of target sedatives in animal tissues. Furthermore, the parameters for the extraction of five sedatives, including the amount of adsorbent, pH value, ion strength, elution solvent and volume, were investigated. Under the optimized conditions, the linear dynamic range was found from 0.1 to 10.0 μg kg^-1, and the limits of detection were ranged from 0.02 to 0.1 μg kg^-1. The method was assessed by the analysis of target sedatives in animal tissues, and the recoveries for the spiked pork muscle and pork liver samples were 84-102% and 83-101%, respectively. The results show that the developed method of PTSPE-LC-MS/MS with ACOPs as adsorbent is efficient for the analysis of trace sedatives in animal tissues.