Application of MIL-53(Al)-NH₂ as a Dispersive Microsolid-Phase Extraction Material for Determination of...

In this paper, an aluminum-based metal-organic framework (MIL-53(Al)-NH₂) was synthesized and employed as a well-known and efficient dispersive microsolid-phase extraction (Dμ-SPE) sorbent for reliable determination of cyclophosphamide in urine samples by the high-performance liquid chromatography (HPLC) technique. The synthesized MIL-53(Al)-NH₂ was characterized by FT-IR, PXRD, FE-SEM, and EDS for more details. Then, the effective parameters of the preconcentration and extraction of urinary cyclophosphamide including the amount of the solid sorbent, the pH of the sample, sample volume, extraction and desorption time, and the type and volume of elution solvent were thoroughly investigated and optimized. According to the results, a linear dynamic range of 0.14-120 μg mL^-1 with a good correlation coefficient (R ² = 0.998) and a limit of detection (LOD) of 0.05 μg mL^-1 were obtained with intra- and interday relative standard deviations (n = 9) of 3.13 and 3.99% in optimized conditions, respectively. Furthermore, the absolute recovery of urinary cyclophosphamide at three concentrations (0.5, 50.0, and 100.0 μg mL^-1) was 94.0%. Finally, the optimal condition of the developed method was successfully applied to the extraction and analysis of cyclophosphamide from the real urine samples with satisfactory recovery (94.0-97.0%) and acceptable precision (<4.1%). The findings proved that MIL-53(Al)-NH₂ can be utilized as a suitable adsorbent for highly reliable extraction of cyclophosphamide in biological matrices.