Application of magnetic solid-phase extraction for sensitive determination of anticancer drugs in urine by means of diamino benzidine tetrachlorohydrate modified magnetic nanoparticles


Pharmacological Reports, vol.75, no.2, pp.456-464, 2023 (SCI-Expanded) identifier identifier identifier

  • Publication Type: Article / Article
  • Volume: 75 Issue: 2
  • Publication Date: 2023
  • Doi Number: 10.1007/s43440-023-00465-5
  • Journal Name: Pharmacological Reports
  • Journal Indexes: Science Citation Index Expanded (SCI-EXPANDED), Scopus, BIOSIS, EMBASE, MEDLINE
  • Page Numbers: pp.456-464
  • Keywords: Paclitaxel, Gemcitabine, Magnetic solid phase extraction, HPLC, Urine samples
  • Erciyes University Affiliated: Yes


Background: The analysis of drug active molecules and residues in the treatment of cancer is important for the sustainability of human life and therapeutic effects. For this purpose, a new magnetic sorbent was developed to use in solid phase extraction prior to conventional high-performance liquid chromatography (HPLC) analysis of Paclitaxel (PAC) and Gemcitabine (GEM) molecules. Methods: In this study, a separation and pre-concentration approach based on magnetic solid phase extraction (MSPE) was proposed for PAC and GEM by means of using a newly synthesized magnetic sorbent. After the MSPE procedure, an HPLC system with a diode array detector (DAD) was used to analyze trace amounts of PAC and GEM anticarcinogenic drugs in urine samples. Surface modification of magnetic Fe3O4 nanoparticles was carried out by diaminobenzidinetetrachloro hydrate (DABTC) for the first time and a useful sorbent was obtained for MSPE experiments. Results: In the proposed method, PAC and GEM molecules were retained on the c in the presence of a pH 5.0 medium and desorbed to 300 μL of acetonitrile: methyl alcohol (1:1) eluent phase before HPLC–DAD analysis. Under the optimized conditions, the limit of detection (LOD) values for PAC and GEM were 1.38 and 1.44 ng mL−1 while the enhancement factor for PAC and GEM were 139.5 and 145.3, respectively. The relative standard deviations (RSD %) for PAC and GEM were below 3.50% in inter-day repeated experiments by means of model solutions containing 100 ng mL−1 drug active ingredients. Conclusions: Synthesis and characterization of DABTC-Fe3O4 nanoparticles were performed using suitable methodologies. Optimization of MSPE was done step by step. And finally, the developed method was successfully applied to urine samples with quantitative recoveries in the range of 99.0% and 105.0%.