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

Yıl 2019, Cilt: 7 Sayı: 2, 434 - 447, 01.06.2019

Ertuğrul Keskin

https://doi.org/10.15317/Scitech.2019.210

Öz

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 L^-1), respectively. Precision and accuracy of the developed
method were checked by recovery studies in spiked tablets and urine.

Anahtar Kelimeler

Adsorptive square wave stripping voltammetry, Cortisol, Glassy carbon electrode, Pharmaceutical formulation, Human urine

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

Öz

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.

Anahtar Kelimeler

Adsorptif kare dalga sıyırma voltametrisi, Kortizol, Camsı karbon elektrot, Farmasötik formülasyon, insan idrarı

Kaynakça

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