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. 2024 Dec;32(2):617-630.
doi: 10.1007/s40199-024-00531-0. Epub 2024 Aug 13.

Dispersive micro-solid phase extraction based on two MOFs as highly effective adsorbents for analysis of nilotinib in plasma and wastewater

Azra Takhvar  1 , Somaye Akbari  1 , Effat Souri  2 , Reza Ahmadkhaniha  3 , Ali Morsali  4 , Mohammad Reza Khoshayand  5 , Mohsen Amini  1 , Alireza Taheri  6
Affiliations

Dispersive micro-solid phase extraction based on two MOFs as highly effective adsorbents for analysis of nilotinib in plasma and wastewater

Azra Takhvar et al. Daru. 2024 Dec.

Abstract

Background: Nilotinib (NIL) is a prescription medication employed in the treatment of specific types of leukemia, namely chronic myelogenous leukemia (CML). The determination of NIL levels in patients undergoing treatment for CML is of paramount importance for effective management of treatment and toxicity. Also, monitoring and controlling its level in wastewater sources could help scientists to identify potential hotspots of contamination and take appropriate measures to mitigate their impact on the environment and public health.

Objectives: This study presents a D-µ-SPE technique utilizing two MOFs as adsorbents for the efficient detection of nilotinib in plasma and wastewater samples for the first time.

Methods: Two highly effective MOFs, MIL-101(Fe) and MIL-53(Al), were synthesized and applied as dispersive micro-solid phase extraction (D-µ-SPE) adsorbents for the extraction of nilotinib coupled with HPLC-UV in a short time of analysis. Experimental parameters affecting extraction efficacy such as adsorbent amount, ionic strength, pH value, adsorption-desorption time and type of elution solvent, were optimized.

Results: Under optimal experimental conditions, the linear dynamic was achieved in the range of 0.25-5.00 µg/mL in human plasma and 0.01-0.20 µg/mL in wastewater. The extraction recovery was in the range of 89.18-91.53% and 94.39-99.60% for nilotinib and MIL-101(Fe) and also 91.22-97.35% and 98.14-100.78% for nilotinib and MIL-53(Al) from human plasma and wastewater respectively.

Conclusion: HPLC-UV determination of nilotinib after the D-µ-SPE method showed acceptable accuracy and precision in both plasma and wastewater. In comparison between the two adsorbents, the extraction procedure was easier and faster with MIL-53(Al) as the adsorbent.

Keywords: Dispersive micro-solid phase extraction; High performance liquid chromatography-ultra violet spectroscopy; MIL101(Fe); MIL53(Al); Nilotinib.

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Conflict of interest statement

Declarations Ethical approval Not applicable. Consent to participate Not applicable. Consent for publication Not applicable Conflict of interest The authors have no relevant financial or non-financial interests to disclose.

Figures

Fig. 1
Fig. 1
Chemical structure of nilotinib hydrochloride monohydrate
Fig. 2
Fig. 2
XRD patterns of MIL-101(Fe) (a) and MIL-53 (Al) (b)
Fig. 3
Fig. 3
FTIR spectra of MIL-101(Fe) (a) and MIL-53 (Al) (b)
Fig. 4
Fig. 4
SEM image of the synthesized MIL-101(Fe) (a), MIL-53(Al) (b)
Fig. 5
Fig. 5
Effect of extraction time (a, b), adsorbent amount (c, d) and ionic strength (e, f)
Fig. 6
Fig. 6
The RSM indicating the effects of adsorbent and time (a), NaCl (%) and time (b) for MIL-101(Fe)
Fig. 7
Fig. 7
The RSM indicating the effects of adsorbent and time (a), NaCl (%) and time (b), and NaCl (%) and adsorbent (c) for MIL-53(Al)
Fig. 8
Fig. 8
Effect of elution solvent (a), desorption time (b) and elution solvent volume (c) on desorption of NIL from MIL-101(Fe) and MIL-53(Al)
Fig. 9
Fig. 9
The HPLC chromatograms of (a) direct injection of blank plasma (b) blank plasma after applying the D-µ-SPE-HPLC–UV(c) spiked plasma after applying the D-µ-SPE-HPLC–UV (nilotinib 1 µg/mL)
See this image and copyright information in PMC

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