Publication: Metilprednisolon aseponat ve benzil alkol’ün yüksek basınçlı sıvı kromatografisi ile yan yana miktar tayin yöntemi geliştirilmesi
Abstract
Amaç: Metilprednisolon aseponatın etken madde olarak kullanıldığı kremlerdeyardımcı madde olarak benzil alkol miktarının fazla tutulmuş olması nedeniylebenzil alkolle birlikte eşzamanlı analizi önemlidir. Bu nedenle çalışmada kremformülasyonlarda eşzamanlı analizi için en uygun yöntemin geliştirilmesi ve ICHkılavuzuna uygun olarak yöntem validasyonu yapılması amaçlanmıştır.Gereç ve yöntem: Kromatografik analizler Poroshell 120 EC-C18 (100x2,1mm2,7μm) kolonla, ACN/ su (39:61 h/ h) karışımı mobil faz olarak kullanılarak izokratikelüsyonla gerçekleştirilmiştir. Akış hızı 0,5 mL/ dk olan metotta DAD dedektör ile245 nm ve 258 nm dalga boyunda çalışılmıştır.Bulgular: Egzama tedavisinde kullanılan kremde MPA ve BA analizi içingeliştirilen HPLC yönteminin core-shell kolonlarda, MPA ve BA’nın yan yanaanalizi için uygun olduğu bulunmuştur. Yöntemin MPA için (0,56x10-7 ve 88,9x10-7)mol/ L BA için (1,4x10-6 ve 33,46x10-6) mol/ L konsantrasyon aralıklarında doğrusalolduğu bulunmuştur.Sonuçlar: Bu yöntem ICH kılavuzuna uyumlu olarak; seçicilik, doğrusallık,doğruluk ve geri kazanılabilirlik, miktar tayin limiti, tanıma limiti, doğruluk, kesinlikve güvenlilik parametreleri ile doğrulanmıştır. Geliştirilen yöntem basit ve hızlıolduğu için kalite kontrol laboratuvarlarında rutin kullanıma uygundur.
Objective: As an excipient benzyl alcohol amount is high in cream formulation ofmethylprednisolone aseponate, thus simultaneous determination of active ingredientmethylprednisolone aseponate and benzyl alcohol is important. Therefore, it is aimedto develop the most suitable method for the simultaneous analysis from creamformulations and to validate the method in accordance with the ICH guidelines.Material and Methods: Choromatographic analysis were performed on a Poroshell120 EC-C18 (100x2.1mm 2.7μm) column using ACN/ water (39:61 v/ v) mixture asmobile phase with a isocratic elution. Flow rate was 0.5 mL/ min, DAD was set at245 nm and 258 nm.Results: HPLC method developed for MPA and BA analysis in eczema treatmentcream was found to be suitable for simultaneous analysis of MPA and BA oncore-shell columns. Calibration curve was linear in the concentration range (0.56x10-7 - 88.9x10- 7) mol/ L for MPA and (1.4x10-6 - 33.46x10-6) mol/ L for BA.Conclusions: The described method was validated for specificity, linearity, limit ofdetection, limit of quantitation, accuracy, precision and robustness as per TheInternational Conference on Harmonisation (ICH) guidelines. All results wereacceptable and this confirmed that the method is suitable for its intended use inroutine quality control and assay of drugs. All results were acceptable and theproposed simple and fast method is suitable for using routine analysis in qualitycontrol laboratories.
Objective: As an excipient benzyl alcohol amount is high in cream formulation ofmethylprednisolone aseponate, thus simultaneous determination of active ingredientmethylprednisolone aseponate and benzyl alcohol is important. Therefore, it is aimedto develop the most suitable method for the simultaneous analysis from creamformulations and to validate the method in accordance with the ICH guidelines.Material and Methods: Choromatographic analysis were performed on a Poroshell120 EC-C18 (100x2.1mm 2.7μm) column using ACN/ water (39:61 v/ v) mixture asmobile phase with a isocratic elution. Flow rate was 0.5 mL/ min, DAD was set at245 nm and 258 nm.Results: HPLC method developed for MPA and BA analysis in eczema treatmentcream was found to be suitable for simultaneous analysis of MPA and BA oncore-shell columns. Calibration curve was linear in the concentration range (0.56x10-7 - 88.9x10- 7) mol/ L for MPA and (1.4x10-6 - 33.46x10-6) mol/ L for BA.Conclusions: The described method was validated for specificity, linearity, limit ofdetection, limit of quantitation, accuracy, precision and robustness as per TheInternational Conference on Harmonisation (ICH) guidelines. All results wereacceptable and this confirmed that the method is suitable for its intended use inroutine quality control and assay of drugs. All results were acceptable and theproposed simple and fast method is suitable for using routine analysis in qualitycontrol laboratories.