Kiral bileşiklerin enansiyomerlerine ayırımı
Küçük Resim Yok
Tarih
2022
Yazarlar
Dergi Başlığı
Dergi ISSN
Cilt Başlığı
Yayıncı
İnönü Üniversitesi
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Amaç: Bu çalışma, mikonazol türevi kiral bileşiklerin enansiyomerlerine ayrımının yapılması ve enansiyomerik saflığı belirlenmesi ile kiral bileşiklerin farmakolojik aktivitelerini ve toksisitelerini değerlendirerek, analitik çalışmaların preparatif çalışmaya uyarlanabileceğini göstermek amacıyla yapılmıştır. Materyal ve metot: Kiral bileşiklerin ayrılması için çeşitli yöntemler bulunur. Bu araştırmada antifungal farmakolojik etkisi olan mikonazol türevi dört farklı bileşiğin kiral ayrımı HPLC cihazı ile yapılmıştır. Sabit faz olarak Chiralpak AD kolonu hareketli faz olarak 0,2 ml/dakika akış hızında çeşitli oranlarda (h/h) metanol-n-hekzan karışımları kullanılarak enansiyomerler ayrılmıştır. Cihaza uyumlu dedektör yardımı ile analizi yapılan maddelerin maksimum absorsiyonda verdikleri dalga boyları tespit edilerek kromatogramlar elde edilmiştir. Bu kromatogramlar sabit fazı tanımamıza yardımcı olan ayırma kapasitesi (k 1 ve k 2 ), selektivite (?), etkinlik (teorik tabaka sayısı, N 1 ve N 2 ) ve rezolüsyon (R s ) kromatografi parametrelerini hesaplamamıza yardımcı olmuştur. Bulgular: Çalışmada kullanılan bileşiklerden ikisi metanol/n-heksan (70:30) mobil faz Chıralpak AD kiral sabit fazda daha iyi ayrım sağlamışken diğer iki bileşik kullanılan kolon ve mobil faz sistemi ile enansiyomer ayrımı gerçekleşmemiştir. Sonuç: Geliştirilen analitik HPLC yöntemi ile elde edilen kromatografik sonuçlar, mikonazol türevi kiral bileşiklerin enansiyomerik ayrımı için optimum koşullar başarılı bir şekilde belirlenmiştir. Ayrıca Chiralpak AD kolonun kiral bileşiklerin preparatif ayrımında da uygulanabileceğini gösterilmiştir.
Aim: This study was carried out to show that analytical studies can be adapted to preparative studies by evaluating the pharmacological activities and toxicities of chiral compounds by separating miconazole derivative chiral compounds into their enantiomers and determining their enantiomeric purity. Material and Method: Various methods exist for the separation of chiral compounds. In this study, chiral separation of four different miconazole derivative compounds with antifungal pharmacological effect was made by HPLC device. The enantiomers were separated by using methanol-n-hexane mixtures at various ratios (v/v) at a flow rate of 0.2 ml/min as the stationary phase with a Chiralpak AD column. With the aid of a detector compatible with the device, the wavelengths of the analyzed substances at maximum absorption were determined and chromatograms were obtained. These chromatograms helped us to calculate the separation capacity (k1 and k2), selectivity (?), efficiency (theoretical layer number, N1 and N2) and resolution (Rs) chromatography parameters that help us to identify the stationary phase. Results: Two of the compounds used in the study, methanol/n-hexane (70:30) mobile phase Chiralpak AD provided better separation in the chiral stationary phase, while the enantiomer separation could not be achieved with the other two compounds using the column and mobile phase system. Conclusion: Chromatographic results obtained by the developed analytical HPLC method, the optimum conditions for the enantiomeric separation of miconazole derivative chiral compounds have been successfully determined. It has also been shown that the Chiralpak AD column can be applied in the preparative separation of chiral compounds.
Aim: This study was carried out to show that analytical studies can be adapted to preparative studies by evaluating the pharmacological activities and toxicities of chiral compounds by separating miconazole derivative chiral compounds into their enantiomers and determining their enantiomeric purity. Material and Method: Various methods exist for the separation of chiral compounds. In this study, chiral separation of four different miconazole derivative compounds with antifungal pharmacological effect was made by HPLC device. The enantiomers were separated by using methanol-n-hexane mixtures at various ratios (v/v) at a flow rate of 0.2 ml/min as the stationary phase with a Chiralpak AD column. With the aid of a detector compatible with the device, the wavelengths of the analyzed substances at maximum absorption were determined and chromatograms were obtained. These chromatograms helped us to calculate the separation capacity (k1 and k2), selectivity (?), efficiency (theoretical layer number, N1 and N2) and resolution (Rs) chromatography parameters that help us to identify the stationary phase. Results: Two of the compounds used in the study, methanol/n-hexane (70:30) mobile phase Chiralpak AD provided better separation in the chiral stationary phase, while the enantiomer separation could not be achieved with the other two compounds using the column and mobile phase system. Conclusion: Chromatographic results obtained by the developed analytical HPLC method, the optimum conditions for the enantiomeric separation of miconazole derivative chiral compounds have been successfully determined. It has also been shown that the Chiralpak AD column can be applied in the preparative separation of chiral compounds.
Açıklama
Anahtar Kelimeler
Eczacılık ve Farmakoloji, Pharmacy and Pharmacology
