Abstract
A Zr-based metal–organic tetrahedron (ZrT-1-NH2) doped monolithic column was sythesized and applied for pipette tip micro solid-phase extraction (PT-μSPE) of 8 phenolic compounds. Scanning electron microscopy, energy dispersive spectrometry, Fourier transform infrared spectroscopy, thermogravimetric analysis and N2 adsorption and desorption experiment were employed to characterize the morphology, composition, structure and thermal stability of the monolithic column. The experimental results showed that the monolithic column had good stability and excellent adsorption selectivity for phenolic compounds. The adsorption mechanism was speculated to be π-π stacking and H-bond interaction based on ESP maps. After the extraction conditions were optimized, a PT-μSPE-high performance liquid chromatography-ultraviolet detector (HPLC-UV) method was established for the detection of 8 phenolic compounds in milk. The PT-μSPE-HPLC-UV method has wide linearities (0.3–1000 μg L−1) (R2 > 0.997), low limits of detection (0.1–0.3 μg L−1), satisfactory recoveries (80.5–113.6 %) and high precision (RSDs < 6.7 %). Thus, the ZrT-1-NH2 doped monolithic column is an ideal medium for the separation and determinaton of phenolic compounds in milk.
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