Related Experiment Video
Updated: Jul 1, 2026

Identifying Inhibitors of the HBx-DDB1 Interaction Using a Split Luciferase Assay System
Published on: December 21, 2019
Nitrogen blowing DµSPE of sunitinib, imatinib, and dasatinib using LDH/MIL-101(Cr)-NO2 composite prior to HPLC-PDA
Hakimeh Mottagi Khosrowshahi1, Jafar Abolhasani1, Mohammad Reza Afshar Mogaddam2,3,4
1Department of Chemistry, Ta.C., Islamic Azad University, Tabriz, Iran.
Background:
The therapeutic bioanalytical challenge activity of tyrosine kinase inhibitors (TKIs) can be assessed by measuring them in biological samples such as plasma and serum. Determining these compounds requires an efficient sample before the analysis to minimize matrix effects and enhance preconcentration. This study presents the use of a composite of layered double hydroxide (LDH) and metal organic framework (MOF) composite for extracting and preconcentrating of sunitinib, imatinib, and dasatinib.
Methodology:
The proposed composite was synthesized through the in-situ growth of MIL-101(Cr)-NO2 MOF on the MgFe-LDH surface. The extraction process involves adding 5 mg of LDH/MIL-101(Cr)-NO2 to the plasma solution containing the analytes, under nitrogen blowing. Centrifugation separated the analyte-loaded sorbent, which was then eluted with 125 μL of mobile phase. The organic phase was used subsequent high performance liquid chromatography (HPLC) - photo diode array detector (PDA) analysis.
Results:
Under optimum conditions, the developed method demonstrates favorable extraction recoveries (66-74%), low limits of detection (LOD) and quantification (LOQ) (0.46-0.69 ng mL-1 and 1.5-2.2 ng mL-1, respectively), wide linear ranges (LRs) (1.5-200 ng mL-1) with high coefficients of determination (0.997-0.999) and proper repeatability (RSD ≤ 6.6%).
Conclusions:
Notably, the method provides the use of minimal amounts of sorbent and solvents, short extraction time, no need for complicated instruments, and high performance in monitoring anti-cancer drugs in biological samples.
Insights
A novel composite of layered double hydroxide (LDH) and metal-organic framework (MOF) efficiently extracts anti-cancer tyrosine kinase inhibitors (TKIs) from biological samples. This method offers a sensitive and rapid approach for bioanalytical monitoring.
Area of Science:
- Analytical Chemistry
- Materials Science
- Pharmacology
Background:
- Tyrosine kinase inhibitors (TKIs) require precise bioanalytical measurement in plasma and serum.
- Efficient sample preparation is crucial to minimize matrix effects and enhance preconcentration for TKI analysis.
- This study addresses the need for improved extraction and preconcentration techniques for TKIs.
Purpose of the Study:
- To develop and validate a composite material for the extraction and preconcentration of specific TKIs.
- To assess the efficacy of a layered double hydroxide (LDH) and metal-organic framework (MOF) composite for TKI analysis.
- To provide a sensitive and efficient method for monitoring anti-cancer drugs in biological matrices.
Main Methods:
- Synthesis of a composite material via in-situ growth of MIL-101(Cr)-NO2 MOF on a MgFe-LDH surface.
- Extraction of sunitinib, imatinib, and dasatinib from plasma using the LDH/MOF composite under nitrogen blowing.
- Analysis of extracted analytes using High-Performance Liquid Chromatography (HPLC) with a Photo Diode Array (PDA) detector.
Main Results:
- The developed method achieved favorable extraction recoveries ranging from 66% to 74%.
- Low limits of detection (LOD) and quantification (LOQ) were obtained (0.46-0.69 ng mL⁻¹ and 1.5-2.2 ng mL⁻¹, respectively).
- The method demonstrated wide linear ranges (1.5-200 ng mL⁻¹) with high coefficients of determination (0.997-0.999) and good repeatability (RSD ≤ 6.6%).
Conclusions:
- The LDH/MOF composite offers a high-performance method for monitoring anti-cancer drugs in biological samples.
- The method utilizes minimal sorbent and solvents, requires short extraction times, and does not need complex instrumentation.
- This approach presents a significant advancement in the bioanalytical challenges associated with TKI quantification.

