POTANSİYEL, V
5. SONUÇ VE ÖNERİLER
Kare dalga voltametrisi son derece hızlı ve duyarlı olma üstünlüğü olan bir puls tekniğidir. Voltamogramın tamamı 10 ms’ den daha kısa bir sürede elde edilir. Tayin alt sınırlarının düşük düzeylere kadar inebilmesi, analizler için herhangi bir ayırma işlemlerine ihtiyaç duyulmaması da diğer üstünlükleri içerisinde yer almaktadır. Bu nedenlerden dolayı tekniğin ilerideki yıllarda çok daha fazla tercih edilecek yöntemlerden biri olacağı düşünülmektedir. Günümüzde KDV tekniği ilaç endüstrisinde klinik ve çevre analizlerinde başta olmak üzere çok çeşitli alanlarda kullanılmaktadır.
Çalışmalarda atorvastatin’ in camsı karbon elektrot üzerindeki elektroanalitik davranışları KDV kullanılarak yükseltgenme yönünde incelenmiştir. Ortamın pH’ının, destek elektrolitinin ve madde derişimlerinin yükseltgenme olayı üzerine etkileri incelenmiştir. Bunun için 0,1 M H2SO4, fosfat tamponları, asetat tamponları ve Britton-Robinson tamponları kullanılmıştır. Yapılan çalışmalar sonucunda seçilen 0,1 M H2SO4 ve pH 3,00 BR tampon çözeltileri içerisinde oldukça pozitif potansiyelde yükseltgenme pikleri elde edilmiştir.
Dönüşümlü voltametri tekniği ile atorvastatin’in pH 3,00 BR tamponu içerisinde 5–1000 mV-1 tarama hızlarında kinetik incelemeleri yapılmıştır. Bu incelemelerde v1/2–Ip ve logv–logIp verileri incelenmiştir. Atorvastatin’ in geri dönüşümsüz ve adsorpsiyonun etkisinde ancak difüzyon kontrollü olarak yükseltgendiği bulunmuştur.
Sonuç olarak atorvastatin’ in tayini için hızlı, kolay, duyarlı, seçici ve herhangi bir ayırma işlemine gerek duyulmayan KDV tekniğinin geliştirilebileceğine karar verilmiştir. Elde edilen bütün veriler ışığında geliştirilecek analiz yönteminin
yeterli doğruluk ve duyarlıkta atorvastatin’in farmasötik dozaj formlarından, serum ve idrar numunelerinden analizinde kullanılabileceği önerilmektedir.
ÖZET
Kare Dalga Voltametrisi ve Uygulamaları
Kare dalga voltametrisi ilaç endüstrisinde, klinik analizlerde ve çevre analizlerinde kullanımı giderek artan oldukça hızlı ve duyarlı bir analitik tekniktir. Basit, hızlı, duyarlı, seçici olması, uzun ve zaman alıcı basamaklara ihtiyaç duymaması gibi nedenlerle de diğer analitik yöntemlerle kıyaslandığında onların alternatifi veya tamamlayıcısı durumundadır.
Çalışmanın deneysel bölümünde atorvastatin kalsiyum’ un elektrokimyasal yükseltgenme davranışı camsı karbon elektrot üzerinde alkol–su karışımı olan ortamda (metanol:su (10:90) (h/h)) pH 1,80–12,00 aralığında kare dalga voltametrisi tekniği kullanılarak incelenmiştir. Deneyler destek elektroliti yapısının, pH’ ın ve tarama hızının reaksiyon üzerindeki etkilerini incelemek amacıyla Britton-Robinson, fosfat, asetat tamponları ve 0,1 M H2SO4 destek elektroliti içerisinde geniş tarama hızı aralığında (5–1000 mVs-1) gerçekleştirilmiştir. Molekül, geri dönüşümsüz ve difüzyon kontrollü olarak yükseltgenmiştir. 0,1 M H2SO4 ve pH 3,00 BR tampon çözeltilerinde molekül oldukça pozitif potansiyellerde elde edilmiş olan yükseltgenme pikleri veya dalgaları ile karakterize edilmiştir. Şartlar optimize edildikten sonra her iki ortamda (pH 3,00 Britton-Robinson tamponu ve 0,1 M H2SO4) akım, 2x10-6 – 8x10-5 M aralığında derişimle doğrusallık göstermiştir.
Anahtar Kelimeler: Kare dalga voltametrisi, atorvastatin kalsiyum, miktar tayini.
SUMMARY
Square wave voltammetry and its applications
Square wave voltammetry is a rapid and sensitive analytical technique which is increasing in utility in the pharmaceutical industry, clinical analysis and environmental analysis. It is used as an alternative or complimentary technique to other analytical methods due to it’ s simplicity, rapidity, sensitivity, selectivity and without any time–consuming preparation compared to other analytical techniques.
Experimental section of this study the electrochemical oxidation of atorvastatin calcium was investigated in hydroalcoholic media ((10:90) methanol:water (v/v)) in pH range 1,80–12,00 using square wave voltammetry at the glassy carbon electrode. To investigate the effects of nature of the supporting electrolyte, pH and scan rate on the anodic reactions were performed in Britton-Robinson, phosphate, acetate buffers 0,1 M H2SO4 and a wide scan rate interval (5−1000 mVs-1). The molecule oxidized irreversibly and by diffusion–controlled. In 0,1 M H2SO4 supporting electrolyte and pH 3,00 BR buffer solution, the molecule was characterized by anodic peaks or wave which were obtained at positive potential.
Under optimized conditions the current showed a linear dependence with concentration in the range between 2x10-6 – 8x10-5 M in both supporting electrolyte (pH 3,00 Britton-Robinson buffer and 0,1 M H2SO4).
Key Words: Square wave voltammetry, atorvastatin calcium, determinations.
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ÖZGEÇMİŞ
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II- Eğitimi
Ankara Üniversitesi Eczacılık Fakültesi …….. 1998-2003 Ankara Çankaya Kılıçaslan Süper Lisesi ……. 1994-1998 Ankara Bahçelievler Deneme Lisesi …..…….. 1991-1994 Ankara Ulubatlı Hasan İlkokulu ……….. 1986-1991 Yabancı dili : İngilizce
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