Farmasötik Formülasyonlarda Roflumilast’ın Türev Spektrofotometrik Yöntem ile Tayini

Year 2016, Issue: 1, 27 - 49, 01.01.2016

Mehmet Atmaca İncilay Süslü

Abstract

Bu çalışmada, farmasötik formülasyonlardaki roflumilastın tayini için basit, hızlı, güvenilir ve tamamen valide edilmiş birinci derece UV spektrofotometrik yöntem geliştirilmiştir. Analiz koşullarını optimize etmek için çözücü tipi, türev derecesi, dalga boyu aralığı ve N değeri test edilmiştir. İlacın kantitatif tayini 190 -350 nm dalga boyu aralığında 220 nm N = 4 ’de birinci türev değerleri kullanılarak yapılmıştır. Geliştirilen yöntem, kararlılık, doğrusallık, duyarlılık, özgünlük, kesinlik, doğruluk, sağlamlık ve tutarlılık açısından valide edilmiştir. Önerilen yöntemin doğrusal olduğu kalibrasyon aralığı 0.75 - 35.00 μg mL-1 ve alt tayin sınırı 0.08 μg mL−1’dir. Geliştirilen ve valide edilen yöntem, farmasötik formulasyonlarındaki roflumilastın tayini için direkt olarak uygulanmıştır. Analiz koşullarında ve seçilen dalga boyunda tablet yardımcı maddelerinden gelen bir girişim bulunmamıştır. Geliştirilen yöntemden elde edilen veriler, literatürdeki yüksek basınçlı sıvı kromatografisi yönteminden elde edilen veriler ile karşılaştırılmış ve iki yöntem arasında istatistiksel olarak anlamlı fark bulunmamıştır. Geliştirilmiş yöntemin duyarlı, doğru, kesin, seçici, sağlam ve tutarlı olduğu sonucuna varılmıştır.

Keywords

Roflumilast, Türev UV spektrofotometri, Optimizasyon, Validasyon, Tablet analizi

Determination of Roflumilast in Pharmaceutical Formulations by Derivative Spectrophotometric Method

Abstract

In this study, a simple, rapid, reliable and fully validated first order derivative UV spectrophotometric method was developed for determination of roflumilast in pharmaceutical formulations. The type of solvent, the degree of derivation, range of wavelength and N value were tested in order to optimize the analysis conditions. The quantitative determination of the drug was carried out using the first - derivative values measured at 220 nm N = 4 in the wavelength range of 190 - 350 nm. The developed method was validated with respect to stability, linearity, sensitivity, specificity, precision, accuracy, robustness and ruggedness. The linear calibration range was found to be 0.75 - 35.00 µg mL-1 and limit of quantitation was 0.08 μg mL−1 for the proposed method. The developed and validated method was directly applied for the determination of roflumilast in its pharmaceutical dosage forms. No interference was found from tablet excipients at the selected wavelength and analysis conditions. The results obtained from the developed method were compared with those obtained by the high performance liquid chromatographic method in the literature and no significant difference was found statistically between two methods. It was concluded that the developed method was sensitive, accurate, precise, selective, robust and rugged.

Keywords

Roflumilast, Derivative UV spectrophotometry, Optimization, Validation, Tablet analysis

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