Paladyum nanoparçacık katkılı karbonsu elektrot üzerinde askorbik asidin voltametrik tayini için yöntem geliştirilmesi

Yıl 2024, Cilt: 13 Sayı: 2, 1 - 10, 31.12.2024

Gamze Çelik , Zafer Üstündağ

https://doi.org/10.17100/nevbiltek.1568250

Öz

Askorbik asit (AA), bağışıklık sistemini destekleme ve oksidatif strese karşı koruma gibi insan sağlığında kritik rolleri olan hayati bir antioksidandır. AA'nın doğru ve hassas bir şekilde belirlenmesi, klinik tanı, farmasötik analiz ve gıda kalite kontrolü için önemlidir. Bu çalışmada, AA tespiti için palladyum katkılı karbonlu malzeme ile modifiye edilmiş camsı karbon (GC) elektrot kullanan yeni bir voltametrik yöntem geliştirilmiştir. Eşit miktarda ham kömür katranı (r-CTP) ve cam elyaf (GF) karışımı, azot atmosferi altında 1000°C'de 1 saat boyunca 10°C/dk ısıtma hızıyla yüksek sıcaklık fırınında piroliz edilmiştir. Elde edilen karbonize malzeme, gezegensel bilyeli öğütücüde (Retsch, PM100) öğütülmüş ve daha sonra üzerine paladyum nanoparçacıkları (PdNP'ler) sol-gel yöntemiyle doplanmıştır. Elde edilen malzeme Pd/CTP-GF olarak adlandırıldı. Pd/CTP-GF, taramalı elektron mikroskobu (SEM) ve X-ışını kırınımı (XRD) yöntemleri ile karakterize edilmiştir. Pd/CTP-GF ile modifiye edilmiş cam karbon (GC) elektrotu
ise dönüşümlü voltametri (CV) ile karakterize edilmiştir. Askorbik asitin tayini için Pd/CTP-GF modifiye edilmiş GC elektrotu üzerinde diferansiyel puls voltametrisi (DPV) kullanılarak bir yöntem geliştirilmiştir. Geliştirilen yöntemin tespit limiti (S/N=3) 5 nM olarak belirlendi. Geliştirilen yöntemin gün içi ve günler arası doğruluk ve kesinliği değerlendirilmiştir. Ayrıca, dopamin, ürik asit ve bazı katyonların askorbik asit üzerindeki interferans etkileri araştırılmıştır. Geliştirilen yöntemin gerçek numune uygulamasında, portakal suyu örneklerinde askorbik asit için %95'in üzerinde bir geri kazanım değeri elde edilmiştir

Anahtar Kelimeler

Askorbik asit, Diferansiyel Puls Voltametrisi, Paladyum Nanoparçacık, Karbonsu Elektrot

Destekleyen Kurum

Doktora tezini destekleyen YÖK 100/2000 ve Tübitak 2211-A burs programlarıdır.

Development of a method for the voltammetric determination of ascorbic acid on a palladium doped carbonaceous electrode

Öz

Ascorbic acid (AA) is a vital antioxidant with critical roles in human health, including immune system support and protection against oxidative stress. Accurate and sensitive determination of AA is essential in clinical diagnostics, pharmaceutical analysis, and food quality control. In this study, a novel voltammetric method was developed using a glassy carbon (GC) electrode modified with palladium-doped carbonaceous material for AA detection. A mixture of equal amounts of raw coal tar pitch (r-CTP) and glass fiber (GF) was pyrolyzed in a high-temperature furnace at 1000°C for 1 h, with a heating rate of 10°C/min under a nitrogen atmosphere. The resulting carbonized material was ground using a planetary ball mill (Retsch, PM100), and palladium nanoparticles (PdNPs) were then doped onto the material via the sol-gel method. The obtained material is denoted Pd/CTP-GF. Pd/CTP-GF was characterized using scanning electron microscopy (SEM) and X-ray diffraction (XRD). The glassy carbon (GC) electrode modified with Pd/CTP-GF was characterized by cyclic voltammetry (CV). A method was developed for the determination of ascorbic acid using differential pulse voltammetry (DPV) on the Pd/CTP-GF modified GC electrode. The detection limit (S/N=3) of the developed method was determined to be 5 nM. The intraday and interday precision and accuracy of the method were also evaluated. In addition, the interference of dopamine, uric acid, and certain cations on ascorbic acid was investigated. In real sample applications, the developed method achieved a recovery of over 95% for ascorbic acid in orange juice samples.
Keywords: Ascorbic acid; differential pulse voltammetry; palladium nanoparticle; carbonaceous electrode.

Anahtar Kelimeler

Ascorbic acid, differential pulse voltammetry, palladium nanoparticle, carbonaceous electrode.

Destekleyen Kurum

YÖK 100/2000 and TUBITAK 2211-A

Teşekkür

In this study, researcher Gamze Çelik was supported by the YÖK-100/2000 and TUBITAK 2111-A scholarship program.

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