Bazı Azol Grubu Antifungal Bileşiklerin Analizi için Ters Faz Sıvı Kromatografi Metot Optimizasyonu

Öz

Bu çalışmada azol türevi antifungal ilaç etken maddeleri klotrimazol, lanokonazol ve klimbazolün ters faz sıvı kromatografi (RPLC) yöntemi kullanılarak geliştirilen metot optimizasyonunda, bileşiklerin kapasite faktörü değerleri ve analizlendikleri hareketli fazdaki metanol derişimi ilişkisi esas alınmıştır. İyonlaşan gruba sahip bu bileşiklerin optimizasyonunda hareketli faz pH değeride optimizasyonda bir diğer etkendir. İzokratik bir ayırma için kapasite faktörü değerlerinin 1-5 aralığında olması tercih edilmektedir. RPLC yöntemiyle gerçekleştirilen klotrimazol, lanokonazol ve klimbazol bileşiklerinin aynı anda tayini için yapılan optimizasyonda %50, %55 ve %60 (v/v) metanol içeren metanol-su ikili karışımları kullanılmıştır. Ayırma için çalışılan ortamlarda iki hareketli faz pH değerindeki (pH 4,0 ve 5,5) alıkonma zamanları belirlenmiştir. Hidrofobik özellikteki bileşiklerin tayini için Zorbax SB-CN (4,6x150mm) kolon tercih edilmiştir. Kolon sıcaklığı 37oC’de ve akış hızı da 1 mL/dakikada sabitlenmiştir. Optimizasyon koşullarının belirlenmesinde logk- % (v/v) metanol ilişkisi ve bileşiklerin ayrılmalarını gösteren seçicilik faktörü (α) parametresinden yararlanılmıştır.

Anahtar Kelimeler

• Antifungal ilaç etken maddeleri
• RPLC
• Metot Optimizasyonu

Reverse Phase Liquid Chromatography Method Optimization for Analysis of Some Azole Group Antifungal Compounds

Öz

In this study, the capacity factor values of the compounds and the methanol concentration in the mobile phase in which they were analyzed were based on the method optimization developed by using the reverse phase liquid chromatography (RPLC) method of the azole antifungal drug active ingredients clotrimazole, lanoconazole and climbazole. In the optimization of these compounds with ionizing groups, the pH value of the mobile phase is another factor in the optimization. For an isocratic separation, it is preferred that the capacity factor values are in the range of 1-5. Methanol-water binary mixtures containing 50%, 55% and 60% (v/v) methanol were used in the optimization for the simultaneous determination of clotrimazole, lanoconazole and climbazol compounds by RPLC method. Retention times at pH values of two mobile phases (pH 4.0 and 5.5) were determined in the working media for separation. Zorbax SB-CN (4.6x150mm) column was preferred for the determination of hydrophobic compounds. The column temperature was fixed at 37 °C and the flow rate was fixed at 1 mL/min. The logk-% (v/v) methanol relationship and the selectivity factor (α) parameter, which shows the separation of the compounds, were used to determine the optimization conditions.

Anahtar Kelimeler

• Antifungal drug active compounds
• RPLC
• Method optimization

Kaynakça

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