Multiple-shell amorphous Co/Ni-(PO4)x(OH)y hollow layered double hydroxide for enhanced extraction of some azole antifungals from biological samples

Antifungals drugs are widely used for variety of fungal infections. Extraction and determination of these drugs in biological sample is crucial because of their toxicity, endocrine-disrupting, and cytochrome P450-mediated effects. In addition, developing an efficient and stable sorbent with a high surface area for microextraction by packed sorbent (MEPS) technique is of great interest. Triple-shell Co/Ni-based hydroxide phosphate (TS-CNHP) was synthesized for increasing surface area. For characterization of TS-CNHP, a combination of advanced analytical methods was employed. Field-emission scanning electron microscopy, transmission electron microscopy, Fourier-transform infrared spectroscopy, Brunauer–Emmett–Teller, dynamic light scattering and X-ray diffraction. In this work the MEPS was coupled with high-performance liquid chromatography equipped with an ultraviolet detector (HPLC-UV). The TS-CNHP demonstrated an impressive level of efficiency and the selectivity for the adsorption of azole antifungals. The optimal conditions for MEPS were determined through a systematic evaluation of key parameters influencing analyte extraction efficiency. These parameters included: pH (6), adsorption time (7 min), adsorption cycles (2 cycles), salt addition (0%), elution solvent (methanol), desorption flow rate (100 µL min^-1), desorption volume (400 µL), and desorption cycles (2 cycles). The analytical performance of the method was thoroughly assessed under optimized conditions. The relative standard deviations (RSDs) ranged from 2.7% to 5.4%, demonstrating a high level of precision. Furthermore, extraction recoveries were observed between 78.0% and 89.7%. A wide linear dynamic range (0.5–1000 μg l^-1) and an acceptable LOD (0.2 µg L⁻¹) for all of the analytes were achieved. The coefficients of determination (R²) of ketoconazole, clotrimazole and miconazole are 0.9985, 0.9986 and 0.9989 respectively, which demonstrating the reliability of the method The proposed MEPS-HPLC-UV technique demonstrates remarkable analytical efficiency in the extraction and quantification of trace levels of azole antifungals from biological matrices, specifically dog and human hair.