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

Year 2024, Volume: 48 Issue: 2, 597 - 607, 20.05.2024

Sercan Yıldırım , Tuğçe Özyiğit

https://doi.org/10.33483/jfpau.1425340

Cited By: 1

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.

Keywords

Antidepresanlar, deneysel tasarım, sıvı kromatografisi

Project Number

1919B012305637

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

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.

Keywords

Antidepressants, design of experiments, liquid chromatography

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.

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