Research Article
BibTex RIS Cite

Sensitive Determination of Gemcitabine Molecule by Novel Magnetic Solid-Phase Extraction Coupled with HPLC-DAD

Year 2025, Volume: 46 Issue: 4, 863 - 869, 30.12.2025
https://doi.org/10.17776/csj.1316184

Abstract

Gemcitabine (GEM) is a widely employed antimetabolite with broad antineoplastic properties and is commonly administered in the treatment of pancreatic, breast, and ovarian cancers. In this study, a new sample preparation and quantification strategy was established to enable the trace-level determination of GEM. The approach integrates magnetic solid-phase extraction (MSPE) with subsequent HPLC–DAD analysis. Within the method, GEM is initially retained on a magnetic sorbent in a pH 5.0 buffer medium, followed by desorption into a reduced volume of ethanol to facilitate chromatographic measurement. Key experimental parameters particularly adsorption and desorption conditions as well as medium pH were systematically examined and optimized. Analytical performance characteristics, including the linear working range, enrichment factor, limit of detection, accuracy, and repeatability, were assessed using model solutions. Chromatographic detection of GEM was achieved at 277 nm under isocratic conditions composed of 60 % methanol, 25 % phosphate buffer at pH 6.0, and 15 % acetonitrile. Partial validation with model solutions demonstrated a detection limit of 3.43 ng mL⁻¹ and an enrichment factor of 100. Overall, the developed method offers high sensitivity, strong reproducibility, and reliable applicability for monitoring GEM at trace concentration levels.

References

  • [1] Rath O., Kozielski F., Kinesins and Cancer, Nat. Rev. Cancer, 12 (2012) 527–539.
  • [2] Xiao M., Li X., Zhang X., Duan X., Lin H., Liu S., Sui G., Assessment of Cancer-Related Signaling Pathways in Responses to Polystyrene Nanoplastics via a Kidney-Testis Microfluidic Platform (KTP), Sci. Total Environ., 857 (2023) 159306.
  • [3] Pantel K., Alix-Panabières C., Riethdorf S., Cancer Micrometastases, Nat. Rev. Clin. Oncol., 6 (2009) 339–351.
  • [4] Nygren P., What is Cancer Chemotherapy? Acta Oncol. (Madr.), 40 (2001) 166–174.
  • [5] Olin J. L., St. Pierre M., Aromatase Inhibitors in Breast Cancer Prevention, Ann. Pharmacother., 48 (2014) 1605–1610.
  • [6] Alping P., Askling J., Burman J., Fink K., Fogdell-Hahn A., Gunnarsson M., Hillert J., Langer-Gould A., Lycke J., Nilsson P., Salzer J., Svenningsson A., Vrethem M., Olsson T., Piehl F., Frisell T., Cancer Risk for Fingolimod, Natalizumab, and Rituximab in Multiple Sclerosis Patients, Ann. Neurol., 87 (2020) 688–699.
  • [7] Borrie A. E., Rose F. A., Choi Y. H., Perera F. E., Read N., Sexton T., Lock M., Vandenberg T. A., Hahn K., Younus J., Logan D., Potvin K., Yaremko B., Yu E., Lenehan J., Welch S., Teft W. A., Kim R. B., Genetic and Clinical Predictors of Arthralgia During Letrozole or Anastrozole Therapy in Breast Cancer Patients, Breast Cancer Res. Treat., 183 (2020) 365–372.
  • [8] Nabholtz J. M., Mouret-Reynier M. A., Durando X., Van Praagh I., Al-Sukhun S., Ferriere J. P., Chollet P., Comparative Review of Anastrozole, Letrozole and Exemestane in the Management of Early Breast Cancer, Expert Opin. Pharmacother., 10 (2009) 1435–1447.
  • [9] Sankar D. G., Latha P. V. M., Kumar B. A., Babu P. J., UV Spectrophotometric Determination of Temozolamide and Gemcitabine, Asian J. Chem., 19(2) (2007) 1605-1607.
  • [10] Parshina N. A., Pleteneva T. V., Baikova V. N., Narimanov M. N., Tyulyandin S. A., Quantitative Estimation of Gemcitabine by HPLC in Plasma, Pharm. Chem. J., (2008) 288-290.
  • [11] Abbruzzese J. L., Grunewald R., Weeks E. A., Gravel D., Adams T., Nowak B., Mineishi S., Tarassoff P., Satterlee W., Raber M. N., Plunkett W., A Phase I Clinical, Plasma, and Cellular Pharmacology Study of Gemcitabine, J. Clin. Oncol., 9 (1991) 491-498.
  • [12] Shen H., Gu Z., Jian K., Qi J., In Vitro Study on the Binding of Gemcitabine to Bovine Serum Albumin, J. Pharm. Biomed. Anal., 75 (2013) 86-93.
  • [13] Lafazanis K., Begas E., Papapostolou I., Iatrou H., Sakellaridis N., Vlassopoulos D., Dimas K., Development and Validation of a Simple and Reliable HPLC-UV Method for Determining Gemcitabine Levels: Application in Pharmacokinetic Analysis, Medicina (Lithuania), 60 (2024) 864.
  • [14] Soni N., Soni N., Ramteke P. W., Pandey H., A Validated RP-HPLC Assay Method for Determination of Gemcitabine Loaded Nanosized Solid Lipid Nanoparticles, J. Drug Deliv. Ther., 8(4) (2018) 308-313.
  • [15] Singh R., Shakya A. K., Naik R., Shalan N., Stability-Indicating HPLC Determination of Gemcitabine in Pharmaceutical Formulations, Int. J. Anal. Chem., 2015 (2015) 62592.
  • [16] Shaik A. H., Kotanka R. R., Singh H., Guru Naidu B., Gandholi S. R., Nalla K., Development and Validation of a Novel Method for the Analysis of Impurities in Gemcitabine Hydrochloride Using RP-HPLC, Journal of Chemical Health Risks, (2024) 14(1), 522-530.
  • [17] Wierucka M., Biziuk M., Application of Magnetic Nanoparticles for Magnetic Solid-Phase Extraction in Preparing Biological, Environmental and Food Samples, TrAC Trends in Analytical Chemistry, 59 (2014) 50-58.
  • [18] Miranda M., Cardoso C., Vitorino C., Fast Screening Methods for the Analysis of Topical Drug Products, Processes, 8(4) (2020) 397.
  • [19] Prata J. C., Sequeira I. F., Monteiro S. S., Silva A. L. P., da Costa J. P., Dias-Pereira P., Fernandes A. J. S., da Costa F. M., Duarte A. C., Rocha-Santos T., Preparation of Biological Samples for Microplastic Identification by Nile Red, Sci. Total Environ., 783 (2021) 147065.
  • [20] Karaca E., Ulusoy S., Morgül U., Ulusoy H. İ., Development of Analytical Method for Sensitive Determination of Streptozotocin Based on Solid Phase Extraction, Cumhuriyet Sci. J., 41 (2020) 826–831.
  • [21] Ulusoy H. İ., Polat U., Ulusoy S., Use of Newly Synthesized Magnetic Fe3O4 Nanoparticles Modified with Hexadecyl Trimethyl Ammonium Bromide for the Sensitive Analysis of Antidepressant Drugs, Duloxetine and Vilazodone, in Wastewater and Urine Samples, RSC Adv., 13 (2023) 20125–20134.
  • [22] Li Q., Lam M. H. W., Wu R. S. S., Jiang B., Rapid Magnetic-Mediated Solid-Phase Extraction and Pre-Concentration of Selected Endocrine Disrupting Chemicals in Natural Waters by Poly(divinylbenzene-co-methacrylic acid) Coated Fe3O4 Core-Shell Magnetite Microspheres for Their Liquid Chromatography, J. Chromatogr. A, 1217 (2010) 1219–1226.
  • [23] Yamini Y., Tahmasebi E., Ranjbar L., Magnetic Nanoparticle-Based Solid-Phase Extraction of Vitamin B12 from Pharmaceutical Formulations, Biol. Trace Elem. Res., 147 (2012) 378–385.
  • [24] Ulusoy H. İ., Yiğit İ. N., Polat Ü., Durgun E., Gürbüzer A., Ulusoy S., Simultaneously HPLC Analysis of B1, B9 and B12 Vitamins at Trace Levels via Cloud Point Extraction, Cumhuriyet Sci. J., 44 (2023) 716–722.
  • [25] De Souza K. C., Andrade G. F., Vasconcelos I., Oliveira Viana I. M., Fernandes C., De Sousa E. M. B., Magnetic Solid-Phase Extraction Based on Mesoporous Silica-Coated Magnetic Nanoparticles for Analysis of Oral Antidiabetic Drugs in Human Plasma, Mater. Sci. Eng. C, 40 (2014) 275–280.
  • [26] Ulusoy H. İ., A Versatile Hydrogel Including Bentonite and Gallocyanine for Trace Rhodamine B Analysis, Colloids Surf. A Physicochem. Eng. Asp., 513 (2017) 110–116.
  • [27] Ulusoy H. İ., Kilit S., Polat Ü., Durgun E., Gürbüzer A., Tümay Özer E., Osman B., Sensitive Analysis of Epilepsy Drug, Phenobarbital, Based on Column Type Solid Phase Extraction and HPLC-DAD System, Cumhuriyet Sci. J., 45 (2024) 763–768.
  • [28] Zhang R., Wang S., Yang Y., Deng Y., Li D., Su P., Yang Y., Modification of Polydopamine-Coated Fe3O4 Nanoparticles with Multi-Walled Carbon Nanotubes for Magnetic-μ-Dispersive Solid-Phase Extraction of Antiepileptic Drugs in Biological Matrices, Anal. Bioanal. Chem., 410(16) (2018) 3779-3788.
  • [29] Durgun E., Ulusoy H. İ., Narin İ., Sensitive, Reliable and Simultaneous Determination of Fingolimod and Citalopram Drug Molecules Used in Multiple Sclerosis Treatment Based on Magnetic Solid Phase Extraction and HPLC-PDA, J. Chromatogr. B Analyt. Technol. Biomed. Life Sci., 1237 (2024) 124071.
  • [30] Temiz, Ş., Ulusoy, S., Ulusoy, H. I., Durgun, E., Polat, U., & Sarp, G., Synthesis and use of new magnetic adsorbent for sensitive, practical and simultaneous analysis Ibuprofen and Ketoprofen molecules in urine samples, Journal of Chromatography B, 1251 (2025) 124404.
  • [31] Altunay N., Elik A., Sarp G., Yılmaz E., Ulusoy H. İ., Tergitol@SiO2@Fe3O4 Magnetic Nano-Material and Experimental Design Methodology: An Effective and Selective Adsorbent for Solid Phase Microextraction and Flame Atomic Absorption Spectrometric Analysis of Lead in Different Matrices, Microchem. J., 170 (2021) 106765.
There are 31 citations in total.

Details

Primary Language English
Subjects Pharmaceutical Analytical Chemistry
Journal Section Research Article
Authors

Halil İbrahim Ulusoy 0000-0002-8742-5145

Nil Beril Alemdar 0009-0009-6723-2467

Songül Ulusoy 0000-0003-3640-5416

Submission Date September 19, 2025
Acceptance Date November 29, 2025
Publication Date December 30, 2025
Published in Issue Year 2025 Volume: 46 Issue: 4

Cite

APA Ulusoy, H. İ., Alemdar, N. B., & Ulusoy, S. (2025). Sensitive Determination of Gemcitabine Molecule by Novel Magnetic Solid-Phase Extraction Coupled with HPLC-DAD. Cumhuriyet Science Journal, 46(4), 863-869. https://doi.org/10.17776/csj.1316184

Editor