Development and Validation of a RPLC Method for the Determination of Capecitabine using Central Composite Design

Abstract

A reversed phase liquid chromatographic (RPLC) method was developed and validated for analysis of capecitabine using central composite design (CCD).The method was optimized using Minitab software with three factors (mobile phase organic modifier concentration, pH of the mobile phase and column temperature). The optimum chromatographic conditions were determined using Derringer's desirability function. The optimum conditions of separation (optimum values of significant factors) determined with the aid of CCD were: (1) mobile phase: The acetonitrile:water binary mixture ratio is 40:60 (%, v/v), (2) column temperature 32oC and (3) pH of the mobile phase is 7.5. The study was carried out on a YMC triart C18(150x4.6 mm I.D, 3m) column and at a flow rate of 1 mL/min.The validation of the developed liquid chromatographic method according to ICH parameters was performed.

Keywords

• Capecitabine,Rivastigmine,Central composite design,Method validation

Merkezi Kompozit Dizayn Kullanılarak Kapesitabin Tayini için RPLC Yönteminin Geliştirilmesi ve Validasyonu

Abstract

Ters faz sıvı kromatografi (RPLC) yöntemi, merkezi kompozit dizayn (CCD) kullanılarak kapesitabinin analizi için geliştirilmiş ve valide edilmiştir. Metot üç faktörle (mobil faz organik modifiyer derişimi, mobil faz pH’sı ve kolon sıcaklığı) Minitab programı kullanılarak optimize edilmiştir. Optimum kromatografik koşullar, Derringer’in istenebilirlik fonksiyonu kullanılarak belirlenmiştir. CCD'nin yardımıyla tayin edilen ayırmanın optimum koşulları: (1) Mobil faz: asetonitril-su ikili karışımı oranı 40:60 (%h/h), (2) kolon sıcaklığı 32oC ve mobil fazın pH'sı 7,5'dur. Çalışma, YMC triart C18 (150x4,6 mm I.D, 3m) kolonda ve 1 mL/dakika akış hızında gerçekleştirilmiştir. Geliştirilen sıvı kromatografik yöntemin ICH parametrelerine göre validasyonu gerçekleştirilmiştir.

Keywords

• Kapesitabin,Rivastigmin,Merkezi kompozit dizayn,Metot validasyonu

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