Application of MIL-53(Al)-NH₂ as a Dispersive Microsolid-Phase Extraction Material for Determination of Cyclophosphamide in Urine by High-Performance Liquid Chromatography

Abstract

In this paper, an aluminum-based metal−organic framework (MIL-53(Al)-NH 2 ) 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)-NH 2 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)-NH 2 can be utilized as a suitable adsorbent for highly reliable extraction of cyclophosphamide in biological matrices.

Developmental toxicity of the emerging contaminant cyclophosphamide and the integrated biomarker response (IBRv2) in zebrafish

“…3 Because of unspecied alkylation (C n H 2n+1 ), CP specically inhibits DNA replication by binding to the molecular structure of DNA, and its affinity to protein molecules is more than 60%. 4 CP under prolonged use or overdosage causes nephrotoxicity, cardiotoxicity, immunotoxicity, gastrointestinal anomalies and kills active ovarian cells to cause cancer in organisms including humans. [5][6][7] Aer consumption by cancer patients, CP and its metabolites (Ndechloroethylcyclophosphamide (DCL-CP), 4-ketocyclophosphamide (4KetoCP), and carboxyphosphamide (CarboxyCP)) are oen released through urine; their concentration in urine samples ranged up to 120 mg/L.…”

“…[5][6][7] Aer consumption by cancer patients, CP and its metabolites (Ndechloroethylcyclophosphamide (DCL-CP), 4-ketocyclophosphamide (4KetoCP), and carboxyphosphamide (CarboxyCP)) are oen released through urine; their concentration in urine samples ranged up to 120 mg/L. 4,8 Depending on their pharmacokinetics, pharmaceuticals (antineoplastic drugs) are released from households, hospital effluents, wastewater from pharmaceutical factories and municipal wastewater. 9 As a result of stable structures, slow degradability and low concentrations pharmaceuticals have not been removed completely in the wastewater treatment plants.…”

Terahertz Spectroscopy Unambiguously Determines the Orientation of Guest Water Molecules in a Structurally Elusive Metal–Organic Framework

“…This absorption-influenced transition is not limited to water alone, as other guest molecules, including CH 4 , N 2 , CO, and O 2 , have been shown to initiate a similar effect. − Additionally, the stability of MIL-53­(Al) under high mechanical stress has also been noted, as it has been reported to undergo a pressure-induced phase transition from its large-pore form to the narrow-pore form at high pressures suggesting its suitability as a nanoshock absorber . Further, MIL-53­(Al) is environmentally and biologically friendly. − Overall, the interesting guest-induced framework dynamics in MIL-53­(Al) are important to understand from a fundamental standpoint, in order to further design and tune the adsorption behavior of host–guest complexes, and this represents a model system for studying the broader class of flexible MOFs.…”

“… 23 Further, MIL-53(Al) is environmentally and biologically friendly. 31 − 33 Overall, the interesting guest-induced framework dynamics in MIL-53(Al) are important to understand from a fundamental standpoint, in order to further design and tune the adsorption behavior of host–guest complexes, and this represents a model system for studying the broader class of flexible MOFs.…”

Preparation of Monolith for Online Extraction and LC–MS Analysis of β-Estradiol in Serum Via a Simple Multicomponent Reaction

“…Various types of materials have been explored, including inorganic, organic, or natural polymers. This includes imprinted materials (MIPs) , and restricted access media, covalent- and metal–organic frameworks (COF and MOF, respectively), hyperporous carbons, carbon materials, ionic liquids . These materials can also be combined into magnetic composites. , …”