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FARMASÖTİK FORMÜLASYONLARDAKİ ANTİDEPRSANLARIN TAYİNİ İÇİN BOX-BEHNKEN TASARIMINA DAYANAN KEMOMETRİK YAKLAŞIM İLE HIZLI SIVI KROMATOGRAFİ YÖNTEMİNİN GELİŞTİRİLMESİ

Year 2024, , 597 - 607, 20.05.2024
https://doi.org/10.33483/jfpau.1425340

Abstract

Amaç: Bu çalışmanın amacı, duloksetin (DXN), fluoksetin (FXN), sitalopram (CIT), paroksetin (PXN) ve sertralin (SRN) adlı antidepresanların tayini için Box-Behnken tasarımına dayalı kemometrik bir yaklaşımla sıvı kromatografik bir yöntem geliştirmektir.
Gereç ve Yöntem: Önemli parametreleri belirlemek için yapılan ilk deneylerden sonra, 17 deney setinden oluşan bir Box-Behnken tasarımı gerçekleştirilmiştir. Tüm ayırma işlemleri bir Agilent Poroshell 120 EC-C18 analitik kolon (75 mm × 4.6 mm × 2.7 µm) kullanılarak gerçekleştirilmiştir.
Sonuç ve Tartışma: pH, asetonitril oranı ve akış hızının optimum seviyeleri, arzu edilebilirlik fonksiyonu ile sırasıyla 2.7, %38.2 ve 1.1 ml/dak olarak belirlenmiştir. Tahmin edilen optimum yanıtlar ile deneysel olarak elde edilen sonuçlar arasındaki farklar (<%8) modelin uygunluğunu kanıtlamıştır. Tespit ve tayin limitleri sırasıyla 0.17-0.29 µg/ml ve 0.53-0.89 µg/ml aralığındadır. Yöntemin uygulanabilirliği, PXN ve DXN'nin formülasyonlarının analiz edilmesiyle kanıtlanmıştır.

Project Number

1919B012305637

References

  • 1. Jia, E., Bartlett, M.G. (2020). Recent advances in liquid chromatographic methods for the determination of selective serotonin reuptake inhibitors and serotonin norepinephrine reuptake inhibitors. Biomedical Chromatography, 34(3), e4760. [CrossRef]
  • 2. Hasin, D.S., Sarvet, A.L., Meyers, J.L., Saha, T.D., Ruan, W.J., Stohl, M., Grant, B.F. (2018). Epidemiology of adult DSM-5 major depressive disorder and its specifiers in the United States. JAMA Psychiatry, 75(4), 336-346. [CrossRef]
  • 3. Fuentes, A.M.A., Fernández, P., Fernández, A.M., Carro, A.M., Lorenzo, R.A. (2019). Microextraction by packed sorbent followed by ultra high performance liquid chromatography for the fast extraction and determination of six antidepressants in urine. Journal of Separation Science, 42(11), 2053-2061. [CrossRef]
  • 4. Hammen, C. (2018). Risk factors for depression: An autobiographical review. Annual Review of Clinical Psychology, 14(1), 1-28. [CrossRef]
  • 5. Dale, E., Bang-Andersen, B., Sánchez, C. (2015). Emerging mechanisms and treatments for depression beyond SSRIs and SNRIs. Biochemical Pharmacology, 95(2), 81-97. [CrossRef]
  • 6. Samanidou, V., Pantazidou, K., Kovatsi, L., Njau, S., Livanos, A. (2012). A simple HPLC method for the simultaneous determination of two selective serotonin reuptake inhibitors and two serotonin-norepinephrine reuptake inhibitors in hair, nail clippings, and cerebrospinal fluid. Journal of Separation Science, 35(7), 839-845. [CrossRef]
  • 7. Stahl, S. M. (1998). Mechanism of action of serotonin selective reuptake inhibitors: Serotonin receptors and pathways mediate therapeutic effects and side effects. Journal of Affective Disorders, 51(3), 215-235. [CrossRef]
  • 8. Salgado-Petinal, C., Lamas, J.P., Garcia-Jares, C., Llompart, M., Cela, R. (2005). Rapid screening of selective serotonin re-uptake inhibitors in urine samples using solid-phase microextraction gas chromatography–mass spectrometry. Analytical and Bioanalytical Chemistry, 382(6), 1351-1359. [CrossRef]
  • 9. Gondová, T., Halamová, D., Špacayová, K. (2008). Simultaneous analysis of new antidepressants by densitometric thin-layer chromatography. Journal of Liquid Chromatography & Related Technologies, 31(16), 2429-2441. [CrossRef]
  • 10. Nouws, H. P. A., Delerue‐Matos, C., Barros, A.A. (2006). Electrochemical determination of citalopram by adsorptive stripping voltammetry-determination in pharmaceutical products. Analytical Letters, 39(9), 1907-1915. [CrossRef]
  • 11. Cârcu-Dobrin, M., Budău, M., Hancu, G., Gagyi, L., Rusu, A., Kelemen, H. (2017). Enantioselective analysis of fluoxetine in pharmaceutical formulations by capillary zone electrophoresis. Saudi Pharmaceutical Journal, 25(3), 397-403. [CrossRef]
  • 12. Dejaegher, B., Vander Heyden, Y. (2011). Experimental designs and their recent advances in set-up, data interpretation, and analytical applications. Journal of Pharmaceutical and Biomedical Analysis, 56(2), 141-158. [CrossRef]
  • 13. Sahu, P.K., Ramisetti, N.R., Cecchi, T., Swain, S., Patro, C.S., Panda, J. (2018). An overview of experimental designs in HPLC method development and validation. Journal of Pharmaceutical and Biomedical Analysis, 147, 590-611. [CrossRef]
  • 14. Hibbert, D.B. (2012). Experimental design in chromatography: A tutorial review. Journal of Chromatography B, 910, 2-13. [CrossRef]
  • 15. Latrous, L. (2022). Optimization and validation in liquid chromatography using design of experiments. Chemistry Africa, 5(3), 437-458. [CrossRef]
  • 16. Yıldırım, S. (2023). A green liquid chromatographic method using ethanol in mobile phase for the determination of nimesulide and naproxen in gel formulations. Turkish Journal of Analytical Chemistry, 5(2), 89-97. [CrossRef]
  • 17. Carlsson, B., Norlander, B. (2001). Optimization and characterization of the chiral separation of citalopram and its demethylated metabolites by response-surface methodology. Chromatographia, 53(5), 266-272. [CrossRef]
  • 18. Hasnain, M.S., Siddiqui, S., Rao, S., Mohanty, P., Jahan Ara, T., Beg, S. (2016). QbD-driven development and validation of a bioanalytical LC-MS method for quantification of fluoxetine in human plasma. Journal of Chromatographic Science, 54(5), 736-743. [CrossRef]
  • 19. Houbart, V., Servais, A.C., Charlier, T.D., Pawluski, J.L., Abts, F., Fillet, M. (2012). A validated microfluidics-based LC-chip-MS/MS method for the quantitation of fluoxetine and norfluoxetine in rat serum. Electrophoresis, 33(22), 3370-3379. [CrossRef]
  • 20. Yıldırım, S., Kadıoğlu, A., Sağlam, A., Yaşar, A., Sellitepe, H.E. (2016). Fast determination of anthocyanins and free pelargonidin in fruits, fruit juices, and fruit wines by high-performance liquid chromatography using a core–shell column. Journal of Separation Science, 39(20), 3927-3935. [CrossRef]
  • 21. de Almeida Borges, V.R., Ribeiro, A.F., de Souza Anselmo, C., Cabral, L.M., de Sousa, V.P. (2013). Development of a high performance liquid chromatography method for quantification of isomers β-caryophyllene and α-humulene in copaiba oleoresin using the Box-Behnken design. Journal of Chromatography B, 940, 35-41. [CrossRef]
  • 22. Mahrouse, M.A., Lamie, N.T. (2019). Experimental design methodology for optimization and robustness determination in ion pair RP-HPLC method development: Application for the simultaneous determination of metformin hydrochloride, alogliptin benzoate and repaglinide in tablets. Microchemical Journal, 147, 691-706. [CrossRef]
  • 23. Taheri, M. (2022). Techno-economical aspects of electrocoagulation optimization in three acid azo dyes’ removal comparison. Cleaner Chemical Engineering, 2, 100007. [CrossRef]
  • 24. Snyder, L.R., Kirkland, J.J., Dolan, J.W. (2010). Introduction to Modern Liquid Chromatography, John Wiley and Sons, p.330-331.
  • 25. Derringer, G., Suich, R. (1980). Simultaneous optimization of several response variables. Journal of Quality Technology, 12(4), 214-219. [CrossRef]

DEVELOPMENT OF A FAST LIQUID CHROMATOGRAPHY METHOD WITH A CHEMOMETRIC APPROACH BASED ON BOX-BEHNKEN DESIGN FOR THE DETERMINATION OF ANTIDEPRESSANTS IN PHARMACEUTICAL FORMULATIONS

Year 2024, , 597 - 607, 20.05.2024
https://doi.org/10.33483/jfpau.1425340

Abstract

Objective: The objective of this work was to develop a liquid chromatographic method for the quantification of antidepressants, namely duloxetine (DXN), fluoxetine (FXN), citalopram (CIT), paroxetine (PXN), and sertraline (SRN), by a chemometric approach based on Box-Behnken design.
Material and Method: After initial experiments to determine significant parameters, a Box-Behnken design consisting of 17 experiment sets was carried out. All separations were conducted using an Agilent Poroshell 120 EC-C18 analytical column (75 mm × 4.6 mm × 2.7 µm).
Result and Discussion: The optimum levels of pH, acetonitrile ratio, and flow rate were determined with the desirability function as 2.7, 38%, and 1.1 ml/min, respectively. The differences (<8%) between predicted optimum responses and experimentally obtained results proved the model's suitability. Limits of detection and limits of quantification values were in the ranges of 0.17-0.29 µg/ml and 0.53-0.89 µg/ml, respectively. The feasibility of the technique was proven by analyzing PXN and DXN formulations.

Supporting Institution

TÜBİTAK

Project Number

1919B012305637

Thanks

T. Özyiğit gratefully acknowledges the financial support from the Research Project Support Programme for Undergraduate Students (2209-A) of The Scientific and Technological Research Council of Turkey.

References

  • 1. Jia, E., Bartlett, M.G. (2020). Recent advances in liquid chromatographic methods for the determination of selective serotonin reuptake inhibitors and serotonin norepinephrine reuptake inhibitors. Biomedical Chromatography, 34(3), e4760. [CrossRef]
  • 2. Hasin, D.S., Sarvet, A.L., Meyers, J.L., Saha, T.D., Ruan, W.J., Stohl, M., Grant, B.F. (2018). Epidemiology of adult DSM-5 major depressive disorder and its specifiers in the United States. JAMA Psychiatry, 75(4), 336-346. [CrossRef]
  • 3. Fuentes, A.M.A., Fernández, P., Fernández, A.M., Carro, A.M., Lorenzo, R.A. (2019). Microextraction by packed sorbent followed by ultra high performance liquid chromatography for the fast extraction and determination of six antidepressants in urine. Journal of Separation Science, 42(11), 2053-2061. [CrossRef]
  • 4. Hammen, C. (2018). Risk factors for depression: An autobiographical review. Annual Review of Clinical Psychology, 14(1), 1-28. [CrossRef]
  • 5. Dale, E., Bang-Andersen, B., Sánchez, C. (2015). Emerging mechanisms and treatments for depression beyond SSRIs and SNRIs. Biochemical Pharmacology, 95(2), 81-97. [CrossRef]
  • 6. Samanidou, V., Pantazidou, K., Kovatsi, L., Njau, S., Livanos, A. (2012). A simple HPLC method for the simultaneous determination of two selective serotonin reuptake inhibitors and two serotonin-norepinephrine reuptake inhibitors in hair, nail clippings, and cerebrospinal fluid. Journal of Separation Science, 35(7), 839-845. [CrossRef]
  • 7. Stahl, S. M. (1998). Mechanism of action of serotonin selective reuptake inhibitors: Serotonin receptors and pathways mediate therapeutic effects and side effects. Journal of Affective Disorders, 51(3), 215-235. [CrossRef]
  • 8. Salgado-Petinal, C., Lamas, J.P., Garcia-Jares, C., Llompart, M., Cela, R. (2005). Rapid screening of selective serotonin re-uptake inhibitors in urine samples using solid-phase microextraction gas chromatography–mass spectrometry. Analytical and Bioanalytical Chemistry, 382(6), 1351-1359. [CrossRef]
  • 9. Gondová, T., Halamová, D., Špacayová, K. (2008). Simultaneous analysis of new antidepressants by densitometric thin-layer chromatography. Journal of Liquid Chromatography & Related Technologies, 31(16), 2429-2441. [CrossRef]
  • 10. Nouws, H. P. A., Delerue‐Matos, C., Barros, A.A. (2006). Electrochemical determination of citalopram by adsorptive stripping voltammetry-determination in pharmaceutical products. Analytical Letters, 39(9), 1907-1915. [CrossRef]
  • 11. Cârcu-Dobrin, M., Budău, M., Hancu, G., Gagyi, L., Rusu, A., Kelemen, H. (2017). Enantioselective analysis of fluoxetine in pharmaceutical formulations by capillary zone electrophoresis. Saudi Pharmaceutical Journal, 25(3), 397-403. [CrossRef]
  • 12. Dejaegher, B., Vander Heyden, Y. (2011). Experimental designs and their recent advances in set-up, data interpretation, and analytical applications. Journal of Pharmaceutical and Biomedical Analysis, 56(2), 141-158. [CrossRef]
  • 13. Sahu, P.K., Ramisetti, N.R., Cecchi, T., Swain, S., Patro, C.S., Panda, J. (2018). An overview of experimental designs in HPLC method development and validation. Journal of Pharmaceutical and Biomedical Analysis, 147, 590-611. [CrossRef]
  • 14. Hibbert, D.B. (2012). Experimental design in chromatography: A tutorial review. Journal of Chromatography B, 910, 2-13. [CrossRef]
  • 15. Latrous, L. (2022). Optimization and validation in liquid chromatography using design of experiments. Chemistry Africa, 5(3), 437-458. [CrossRef]
  • 16. Yıldırım, S. (2023). A green liquid chromatographic method using ethanol in mobile phase for the determination of nimesulide and naproxen in gel formulations. Turkish Journal of Analytical Chemistry, 5(2), 89-97. [CrossRef]
  • 17. Carlsson, B., Norlander, B. (2001). Optimization and characterization of the chiral separation of citalopram and its demethylated metabolites by response-surface methodology. Chromatographia, 53(5), 266-272. [CrossRef]
  • 18. Hasnain, M.S., Siddiqui, S., Rao, S., Mohanty, P., Jahan Ara, T., Beg, S. (2016). QbD-driven development and validation of a bioanalytical LC-MS method for quantification of fluoxetine in human plasma. Journal of Chromatographic Science, 54(5), 736-743. [CrossRef]
  • 19. Houbart, V., Servais, A.C., Charlier, T.D., Pawluski, J.L., Abts, F., Fillet, M. (2012). A validated microfluidics-based LC-chip-MS/MS method for the quantitation of fluoxetine and norfluoxetine in rat serum. Electrophoresis, 33(22), 3370-3379. [CrossRef]
  • 20. Yıldırım, S., Kadıoğlu, A., Sağlam, A., Yaşar, A., Sellitepe, H.E. (2016). Fast determination of anthocyanins and free pelargonidin in fruits, fruit juices, and fruit wines by high-performance liquid chromatography using a core–shell column. Journal of Separation Science, 39(20), 3927-3935. [CrossRef]
  • 21. de Almeida Borges, V.R., Ribeiro, A.F., de Souza Anselmo, C., Cabral, L.M., de Sousa, V.P. (2013). Development of a high performance liquid chromatography method for quantification of isomers β-caryophyllene and α-humulene in copaiba oleoresin using the Box-Behnken design. Journal of Chromatography B, 940, 35-41. [CrossRef]
  • 22. Mahrouse, M.A., Lamie, N.T. (2019). Experimental design methodology for optimization and robustness determination in ion pair RP-HPLC method development: Application for the simultaneous determination of metformin hydrochloride, alogliptin benzoate and repaglinide in tablets. Microchemical Journal, 147, 691-706. [CrossRef]
  • 23. Taheri, M. (2022). Techno-economical aspects of electrocoagulation optimization in three acid azo dyes’ removal comparison. Cleaner Chemical Engineering, 2, 100007. [CrossRef]
  • 24. Snyder, L.R., Kirkland, J.J., Dolan, J.W. (2010). Introduction to Modern Liquid Chromatography, John Wiley and Sons, p.330-331.
  • 25. Derringer, G., Suich, R. (1980). Simultaneous optimization of several response variables. Journal of Quality Technology, 12(4), 214-219. [CrossRef]
There are 25 citations in total.

Details

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

Sercan Yıldırım 0000-0003-2457-8248

Tuğçe Özyiğit 0000-0003-2058-0551

Project Number 1919B012305637
Early Pub Date April 25, 2024
Publication Date May 20, 2024
Submission Date January 25, 2024
Acceptance Date April 1, 2024
Published in Issue Year 2024

Cite

APA Yıldırım, S., & Özyiğit, T. (2024). DEVELOPMENT OF A FAST LIQUID CHROMATOGRAPHY METHOD WITH A CHEMOMETRIC APPROACH BASED ON BOX-BEHNKEN DESIGN FOR THE DETERMINATION OF ANTIDEPRESSANTS IN PHARMACEUTICAL FORMULATIONS. Journal of Faculty of Pharmacy of Ankara University, 48(2), 597-607. https://doi.org/10.33483/jfpau.1425340
AMA Yıldırım S, Özyiğit T. DEVELOPMENT OF A FAST LIQUID CHROMATOGRAPHY METHOD WITH A CHEMOMETRIC APPROACH BASED ON BOX-BEHNKEN DESIGN FOR THE DETERMINATION OF ANTIDEPRESSANTS IN PHARMACEUTICAL FORMULATIONS. Ankara Ecz. Fak. Derg. May 2024;48(2):597-607. doi:10.33483/jfpau.1425340
Chicago Yıldırım, Sercan, and Tuğçe Özyiğit. “DEVELOPMENT OF A FAST LIQUID CHROMATOGRAPHY METHOD WITH A CHEMOMETRIC APPROACH BASED ON BOX-BEHNKEN DESIGN FOR THE DETERMINATION OF ANTIDEPRESSANTS IN PHARMACEUTICAL FORMULATIONS”. Journal of Faculty of Pharmacy of Ankara University 48, no. 2 (May 2024): 597-607. https://doi.org/10.33483/jfpau.1425340.
EndNote Yıldırım S, Özyiğit T (May 1, 2024) DEVELOPMENT OF A FAST LIQUID CHROMATOGRAPHY METHOD WITH A CHEMOMETRIC APPROACH BASED ON BOX-BEHNKEN DESIGN FOR THE DETERMINATION OF ANTIDEPRESSANTS IN PHARMACEUTICAL FORMULATIONS. Journal of Faculty of Pharmacy of Ankara University 48 2 597–607.
IEEE S. Yıldırım and T. Özyiğit, “DEVELOPMENT OF A FAST LIQUID CHROMATOGRAPHY METHOD WITH A CHEMOMETRIC APPROACH BASED ON BOX-BEHNKEN DESIGN FOR THE DETERMINATION OF ANTIDEPRESSANTS IN PHARMACEUTICAL FORMULATIONS”, Ankara Ecz. Fak. Derg., vol. 48, no. 2, pp. 597–607, 2024, doi: 10.33483/jfpau.1425340.
ISNAD Yıldırım, Sercan - Özyiğit, Tuğçe. “DEVELOPMENT OF A FAST LIQUID CHROMATOGRAPHY METHOD WITH A CHEMOMETRIC APPROACH BASED ON BOX-BEHNKEN DESIGN FOR THE DETERMINATION OF ANTIDEPRESSANTS IN PHARMACEUTICAL FORMULATIONS”. Journal of Faculty of Pharmacy of Ankara University 48/2 (May 2024), 597-607. https://doi.org/10.33483/jfpau.1425340.
JAMA Yıldırım S, Özyiğit T. DEVELOPMENT OF A FAST LIQUID CHROMATOGRAPHY METHOD WITH A CHEMOMETRIC APPROACH BASED ON BOX-BEHNKEN DESIGN FOR THE DETERMINATION OF ANTIDEPRESSANTS IN PHARMACEUTICAL FORMULATIONS. Ankara Ecz. Fak. Derg. 2024;48:597–607.
MLA Yıldırım, Sercan and Tuğçe Özyiğit. “DEVELOPMENT OF A FAST LIQUID CHROMATOGRAPHY METHOD WITH A CHEMOMETRIC APPROACH BASED ON BOX-BEHNKEN DESIGN FOR THE DETERMINATION OF ANTIDEPRESSANTS IN PHARMACEUTICAL FORMULATIONS”. Journal of Faculty of Pharmacy of Ankara University, vol. 48, no. 2, 2024, pp. 597-0, doi:10.33483/jfpau.1425340.
Vancouver Yıldırım S, Özyiğit T. DEVELOPMENT OF A FAST LIQUID CHROMATOGRAPHY METHOD WITH A CHEMOMETRIC APPROACH BASED ON BOX-BEHNKEN DESIGN FOR THE DETERMINATION OF ANTIDEPRESSANTS IN PHARMACEUTICAL FORMULATIONS. Ankara Ecz. Fak. Derg. 2024;48(2):597-60.

Kapsam ve Amaç

Ankara Üniversitesi Eczacılık Fakültesi Dergisi, açık erişim, hakemli bir dergi olup Türkçe veya İngilizce olarak farmasötik bilimler alanındaki önemli gelişmeleri içeren orijinal araştırmalar, derlemeler ve kısa bildiriler için uluslararası bir yayım ortamıdır. Bilimsel toplantılarda sunulan bildiriler supleman özel sayısı olarak dergide yayımlanabilir. Ayrıca, tüm farmasötik alandaki gelecek ve önceki ulusal ve uluslararası bilimsel toplantılar ile sosyal aktiviteleri içerir.