YALIN CAMSI KARBON ELEKTROT KULLANARAK FARMASÖTİK FORMULASYON VE İNSAN İDRARINDAN KORTİZOLÜN HIZLI KARE DALGA VOLTAMETRİK ANALİZİ

Ticari ilaçlardan ve insan idrarından kortizolün direkt tayini için basit, hızlı ve duyarlı bir elektrokimyasal yöntem geliştirildi. Kortizolün elektrokimyasal indirgenmesi ve nicel analizleri, dönüşümlü voltametri (DV) ve kare dalga voltametrisi (KDV) kullanılarak yalın camsı karbon elektrot (CKE) ile Britton-Robinson tampon çözeltisinde (BRTÇ) ve pH 2,0’de gerçekleştirildi. Kortizol DV’de, tersinmez ve adsorpsiyon kontrollü bir indirgeme piki gösterdi. Adsorptif kare dalga sıyırma voltametrisi (Ad-KDSV) kullanıldığında bileşik BRTÇ pH 2,0 içinde ve -1,14 V'de (Ag/AgCl'ye karşı) iyi tanımlanmış bir voltametrik yanıt verdi. Deneysel sonuçlar pik akımı ile 1-50 µg mL-1 (2,8x10-6 mol L-1 - 4×10-4 mol L-1 ) derişim aralığında doğrusal bir ilişki olduğunu ortaya koymuştur. Gözlenebilirlik sınırı (GS) ve tayin alt sınırı (TAS) sırasıyla 0,069 µg mL-1 (1,9×10-7 mol L-1 ) ve 0,229 µg mL-1 (6,32×10-7 mol L-1 ) olarak saptandı. Geliştirilen yöntemin kesinliği ve doğruluğu, tablet ve idrar numunelerinden yapılan geri kazanım çalışmaları ile kontrol edildi.

FAST SQUARE WAVE VOLTAMMETRIC DETERMINATION OF CORTISOL IN PHARMACEUTICAL FORMULATION AND HUMAN URINE USING THE BARE GLASSY CARBON ELECTRODE

A simple, fast and sensitive electrochemical method for the direct determination of cortisol in commercial pharmaceutical product and human urine was developed. The electrochemical reduction and quantitative analysis of cortisol were performed in Britton Robinson Buffer Solution (BRBS, pH 2.0) with a bare glassy carbon electrode (GCE) using cyclic voltammetry (CV) and square wave voltammetry (SWV). The compound showed one irreversible and adsorption-controlled reduction peak in CV. When SWSV mode is used, the compound yielded a well-defined voltammetric response at about -1.14 V (vs. Ag/AgCl) in BRBS at pH 2.0. Experimental results revealed an excellent linear correlation between the peak current and the concentration in the range of 1-50 µg mL-1 (2.8×10-6 -1.4×10-4 mol L-1 ). Detection and quantification limits were found to be 0.069 µg mL-1 (1.9×10-7 mol L-1 ) and 0.229 µg mL-1 (6.32×10-7 mol L1 ), respectively. Precision and accuracy of the developed method were checked by recovery studies in spiked tablets and urine.

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