Farmasötik Şekillerde Galantamin Miktarının Belirlenmesi İçin Alternatif Analitik Yöntemler

Abstract

Amaç: Galantaminin yığın halinde ve farmasötik dozaj formunda miktar tayini için, yeni seçici, hızlı, kesin ve doğru spektrofotometrik ve kromatografik prosedürler geliştirildi ve doğrulandı.

Gereç ve Yöntem: Kromatografik ayırma, bir Agilent Extend C18 (250x4.6 mm, 5 um) kolonu üzerinde gerçekleştirilmiştir. %0,1 TFA içeren ultra saf su ve %0,1 TFA içeren asetonitril (85/15, v/v) 1.0 mL/dk akış hızında mobil faz olarak kullanıldı. Eluent tespiti, bir UV detektörü kullanılarak 288 nm dalga boyunda gerçekleştirilmiştir. Galantamin ise 288 nm dalga boyunda çözeltilerin absorbansı ölçülerek spektrofotometrik teknikle belirlendi.

Bulgular: Galantamin için Lambert−Beer grafikleri, 5-30 μg/mL konsantrasyon aralığında doğrusal ilişkiler gösterdi. Her iki teknik de Uluslararası Uyumlaştırma Konferansı (ICH) standartlarını karşılamak için istatistiksel olarak değerlendirilmiş ve doğrulanmıştır ve sonuçlar, spektrofotometrik ve sıvı kromatografik yöntemlerin doğrusal, hassas, doğru, sağlam ve RSD değerlerinin %1,00'dan düşük olduğunu göstermiştir. ve geri kazanım yüzdesi standart sınırlar içindeydi (%98-102). Daha sonra bu analitik yöntemlerin istatistiksel bir karşılaştırması yapıldı. Her iki yöntemin sonuçları da %95 güven aralığında (p<0,05) birbirlerine göre farklılık göstermedi ve istatistiksel olarak anlamlı değildi.

Sonuç: Geliştirilen analitik yöntemlerin doğru, oldukça etkili, güvenilir, hızlı, basit olduğu belirlendi ve farmasötik dozaj formunun yanı sıra yığın halindeki galantaminin rutin analizi için başarıyla kullanılabilir. Kalite kontrol analizi ve temizlik doğrulaması sırasında numune analizi için bile kullanılabilirler.

Keywords

• Galantamin
• HPLC
• UV
• Yöntem
• Validasyon

Alternative Analytical Methods for Quantification of Galantamine in Pharmaceuticals

Abstract

Objective: For the quantification of galantamine in bulk and pharmaceutical dosage form, new selective, quick, precise, and accurate spectrophotometric and chromatographic procedures were developed and validated.

Material & Methods: Chromatographic separation was performed on an Agilent Extend C18 (250×4.6 mm, 5 µm) column. Ultrapure water containing 0.1% TFA and acetonitrile containing 0.1% TFA (85/15, v/v) were used as mobile phase at a flow rate of 1.0 mL/min. Eluent detection was performed at a wavelength of 288 nm using a UV detector. On the other hand, galantamine was determined by spectrophotometric technique by measuring the absorbance of the solutions at a wavelength of 288 nm.

Result: Lambert−Beer plots for galantamine showed linear relationships in the concentration range of 5-30 μg/mL. Both techniques have been statistically evaluated and validated in order to meet the standards of the International Conference on Harmonisation (ICH) and the results showed that spectrophotometric and liquid chromatographic methods were linear, precise, accurate, rugged and robust with RSD values less than 1.00%, and the recovery percentage was within standard limits (98-102%). Then a statistical comparison of these analytical methods was performed. The results of both methods showed no difference and not statistically significant with respect to each other in the 95% confidence interval (p<0.05).

Conclusion: The developed analytical methods were determined to be accurate, highly effective, reliable, fast, simple, and may be employed successfully for routine analysis of galantamine in the bulk as well as pharmaceutical dosage form. They may even be used for quality control analysis and for sample analysis during cleaning validation.

Keywords

• Galantamine
• HPLC
• UV
• Method
• Validation

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