Simultaneous determination of raloxifene and tamoxifen using dispersive micro solid-phase extraction and HPLC method in real water, human hair and serum samples

ABSTRACT

A sensitive determination procedure was presented for two anticancer drugs (tamoxifen and raloxifene) in real water and biological samples based on magnetic dispersive micro solid-phase extraction–high-performance liquid chromatography with an ultraviolet detector. Fe₃O₄ NPs@SiO₂@TiO₂ nanocomposite was synthesised as a magnetic sorbent by the sol-gel technique. The effective parameters in the procedure were optimised with an experimental design, including screening and optimisation steps. Under the optimum determination conditions, the procedure displayed wide linear ranges of 5.3–735.0 and 7.0–806.0 ng mL⁻¹ with R-squared of 0.9916 and 0.9908, limit of detections of 1.6 and 2.1 ng mL⁻¹ for the raloxifene and tamoxifen determination, respectively. The intra-day relative standard deviations were 3.76 and 3.59% for three times the raloxifene and tamoxifen measurements, respectively. The preconcentration factors for the raloxifene and tamoxifen determination with a concentration of 20 ng mL⁻¹ were 506.1 and 546.7, respectively. The method was applied to analyse well water, tap water, and hair samples and determine raloxifene and tamoxifen simultaneously with recoveries between 88.5–96.4 and relative standard deviations lower than 8.4%. The method’s advantages for raloxifene and tamoxifen measurement included easy operation, low sorbent and desorption solvent consumption, simple sorbent preparation and separation, and suitable analysis time.

KEYWORDS:

• Tamoxifen
• raloxifene
• dispersive micro solid-phase extraction
• hair sample
• real water sample
• experimental design

Acknowledgments

The authors gratefully acknowledge this research’s support from the Islamic Azad University of Mashhad, Iran.

Disclosure statement

The authors confirm that there are no known conflicants of interest related to this publication article.

Data availability statement

All data generated or analysed during this study are included in this published article and its supplementary information files.

Ethical approval

All procedures performed in this study involving human participants were in accordance with the ethical standards and human rights guidelines mentioned in the “Ethical Principles for Medical Research ‘Involving Human Subjects’ of the ‘World Medical Association’. The Ethics Committee of Islamic Azad University of Mashhad approved this study.

Informed consent

The human real samples were obtained from the donator volunteers who signed the informed consent form prepared for individuals.

Supplementary material

Supplemental data for this article can be accessed online at https://doi.org/10.1080/03067319.2022.2118054