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

Öz

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.

Anahtar Kelimeler

• Antidepressants
• design of experiments
• liquid chromatography

Destekleyen Kurum

TÜBİTAK

Proje Numarası

1919B012305637

Teşekkür

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.

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

Öz

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.

Anahtar Kelimeler

• Antidepresanlar
• deneysel tasarım
• sıvı kromatografisi

Proje Numarası

1919B012305637

Kaynakça

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