ZERO-ORDER AND FIRST-DERIVATIVE SPECTROPHOTOMETRY FOR THE DETERMINATION OF SPIRONOLACTONE IN PHARMACEUTICAL TABLETS

Year 2025, Volume: 49 Issue: 3, 672 - 680, 19.09.2025

Asiye Üçer , Nezaket Başaran , Erdal Dinç , Özgür Üstündağ

https://doi.org/10.33483/jfpau.1608315

Abstract

Objective: Spironolactone, a potassium-sparing diuretic drug on the WHO's Essential Medicines List, is primarily used to treat fluid retention resulting from heart failure, kidney disease, and liver scarring. In this research article, zero-order, and first-derivative spectrophotometric approaches were applied to the quantity of spironolactone in pharmaceutical tablet formulation without any separation procedure.
Material and Method: Spironolactone compound was obtained from Sigma-Aldrich (Steinheim, Germany). As a solvent methanol (J.T. Baker, Netherlands, HPLC grade) was used for UV-visible spectrophotometric assays. In the implementation of the zero-order and first-derivative approaches, the quantification of Spironolactone was carried out using UV spectrophotometric measurements in the 200-300 nm wavelength range (with a 2 nm increment) and 1 cm quartz cells. These approaches were tested by analyzing spironolactone in independent test samples and spiked samples. The tablet analyses of spironolactone were performed on ALDACTONE®-A 25 mg Tablet supplied by Aris Ali Raif Pharmaceuticals Industry, Başakşehir, İstanbul, Türkiye.
Result and Discussion: The analysis of spironolactone was conducted using zero-order values measured at 239 nm and first-derivative values measured at 250.4 nm (n=3). The calibration graphs created at these wavelengths showed linearity within the 6.0 to 20.0 µg/ml concentration range, with correlation coefficients of r = 0.9996 for the zero-order method and r = 0.9997 for the first-order derivative method. The validity of the methods was proved by analyzing spironolactone in independent test samples and spiked samples. These methods were then applied to the quantitation of spironolactone in commercial tablets and a good agreement was reported between label claim assay results.

Keywords

Antihyypertensive drug , determination of spironolactone , first derivative spectrophotometry , tablet analysis , zero-order spectrophotometry

Supporting Institution

This work was carried out at the Chemometric Laboratory of Ankara University, Faculty of Pharmacy funded by the scientific research project number 10A3336001.

Project Number

10A3336001

FARMASÖTİK TABLETLERDEKİ SPİRONOLAKTONUN TAYİNİ İÇİN SIFIR DERECEDEN VE BİRİNCİ TÜREV SPEKTROFOTOMETRİ

Abstract

Amaç: WHO'nun Temel İlaçlar Listesi'nde yer alan potasyum tutucu bir diüretik ilaç olan spironolakton, öncelikli olarak kalp yetmezliği, böbrek hastalığı ve karaciğer skarlaşmasından kaynaklanan sıvı tutulumunu tedavi etmek için kullanılır. Bu araştırma makalesinde, herhangi bir ayırma prosedürü olmaksızın farmasötik tablet formülasyonundaki spironolakton miktarına sıfırıncı mertebeden ve birinci türev spektrofotometrik yaklaşımlar uygulandı.
Gereç ve Yöntem: Spironolakton bileşiği Sigma-Aldrich'ten (Steinheim, Almanya) elde edildi. Çözücü olarak metanol (J.T. Baker, Hollanda, HPLC sınıfı) UV-görünür spektrofotometrik analizler için kullanıldı. Sıfırıncı mertebe ve birinci türev yaklaşımlarının uygulanmasında, Spironolaktonun kantifikasyonu 200-300 nm dalga boyu aralığında (2 nm artışla) ve 1 cm kuvars hücrelerde UV spektrofotometrik ölçümler kullanılarak gerçekleştirildi. Bu yaklaşımlar, spironolaktonun bağımsız test örneklerinde ve spike edilmiş örneklerde analiz edilmesiyle test edildi. Spironolaktonun tablet analizleri, Aris Ali Raif İlaç Sanayi, Başakşehir, İstanbul, Türkiye tarafından tedarik edilen ALDACTONE®-A 25 mg Tablet üzerinde gerçekleştirildi.
Sonuç ve Tartışma: Spironolakton analizi, 239 nm'de ölçülen sıfırıncı mertebeden değerler ve 250,4 nm'de ölçülen birinci türev değerleri kullanılarak gerçekleştirildi (n=3). Bu dalga boylarında oluşturulan kalibrasyon grafikleri, sıfırıncı mertebeden yöntem için r = 0,9996 ve birinci mertebeden türev yöntemi için r = 0,9997 korelasyon katsayılarıyla 6,0 ila 20,0 µg/ml konsantrasyon aralığında doğrusallık gösterdi. Yöntemlerin geçerliliği, bağımsız test örneklerinde ve güçlendirilmiş örneklerde spironolaktonun analiz edilmesiyle kanıtlandı. Daha sonra bu yöntemler ticari tabletlerdeki spironolaktonun kantifikasyonuna uygulandı ve etiket iddiası deney sonuçları arasında iyi bir uyum bildirildi.

Keywords

Antihipertansif ilaç , birinci türev spektrofotometri , sıfırıncı mertebe spektrofotometri , spironolakton tayini , tablet analizi

Project Number

10A3336001

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