Triamsınolon asetonidin elektrokimyasal davranışı ve ilaç formlarından HPLC ile analizi
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Tarih
2019
Yazarlar
Dergi Başlığı
Dergi ISSN
Cilt Başlığı
Yayıncı
Çanakkale Onsekiz Mart Üniversitesi
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Triamsinolon Asetonid'in (TA) voltametrik tekniklerle elektrokimyasal davranışı, Yüsek Performanslı Sıvı Kromatografisi (HPLC) tekniğiyle ise ilaç formlarındaki miktarı belirlenmiştir. Elektrokimyasal deneyler kalem ucu grafit elektrotta (KUGE) 0.50-12.00 pH arasındaki çeşitli tampon çözeltiler kullanarak Döngüsel Voltametri (CV) ve Diferensiyel PulsVoltametrisi (DPV) metodlarıyla gerçekleştirilmiştir. Kromatografik deneyler ise C18 analitik kolon ile 25oC'de ve 254 nm'de gerçekleştirilmiştir. TA'nın çalışma ortamını belirlemek için farklı destek elektrolitlerde pH'ın pik potansiyeline ve pik akımına etkisi incelenmiştir. Yüksek akımın ve en iyi pikin gözlendiği Britton-Robinson tampon çözeltisi (pH 3.50) seçilmiştir. CV ölçümlerinden elde edilen tarama hızının karekökü-akım değerleri ve log v-logi grafiklerinden, akımın adsorpsiyon kontrollü olduğu tespit edilmiştir. Gercek ilaç numunelerinde TA'nın miktarı HPLC tekniği ile belirlenmiştir. Bu amaçla TA' nın 2,3x10-7 – 1,15x10-4 derişim aralığında HPLC yöntemi ile lineer bir kalibrasyon doğrusu oluşturulmuştur. Bu kalibrasyon grafiği kullanılarak belirme sınırı ve kantitatif tayin sınırı sırasıyla 3,92x10-8 ve 1,29x10-7 olarak bulunmuştur. Daha sonra TA'nın ilaç formlarındaki miktarı belirlenmiştir. Gerçek ilaç numunlerine uygulanan HPLC metodunun validasyonu da yapılmıştır.
The electrochemical behavior of triamcinolone acetonide (TA) was determined by voltammetric techniques and the amount of itsin the drug form was determined by High Performance Liquid Chromatography (HPLC) technique. Electrochemical experiments were carried out by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methods in Various Buffer in the pH 0.50-12.00 on the pen-tip graphite electrode (KUGE). Chromatographic experiments were performed with C18 analytical column at 25oC and 254 nm. In order to determine the experimental conditationof TA, the effect of pH on peak potential and peak current in different electrolytes were investigated. Britton-Robinson buffer (pH 3.50), where high current and best peak was observed, was selected as support electrolyte and pH. From the square root-of the scane rate-current and the log scane rate-log current graphsobtained from CV measurements, it was determined that the current was adsorption controlled.The amount of TA in the actual drug samples was determined by HPLC technique. For this purpose, a linear calibration curve was formed by HPLC technique in the concentration range of 2,3x10-7 - 1,15x10-4. Using this calibration graph, the detection limit (LOD) and quantitative determination limit (LOQ) were found to be 3.92x10-8 and 1.29x10-7, respectively. Then, the amount of TA from the drug forms was determined. The validation of the HPLC method applied to the actual drug samples was also performed.
The electrochemical behavior of triamcinolone acetonide (TA) was determined by voltammetric techniques and the amount of itsin the drug form was determined by High Performance Liquid Chromatography (HPLC) technique. Electrochemical experiments were carried out by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methods in Various Buffer in the pH 0.50-12.00 on the pen-tip graphite electrode (KUGE). Chromatographic experiments were performed with C18 analytical column at 25oC and 254 nm. In order to determine the experimental conditationof TA, the effect of pH on peak potential and peak current in different electrolytes were investigated. Britton-Robinson buffer (pH 3.50), where high current and best peak was observed, was selected as support electrolyte and pH. From the square root-of the scane rate-current and the log scane rate-log current graphsobtained from CV measurements, it was determined that the current was adsorption controlled.The amount of TA in the actual drug samples was determined by HPLC technique. For this purpose, a linear calibration curve was formed by HPLC technique in the concentration range of 2,3x10-7 - 1,15x10-4. Using this calibration graph, the detection limit (LOD) and quantitative determination limit (LOQ) were found to be 3.92x10-8 and 1.29x10-7, respectively. Then, the amount of TA from the drug forms was determined. The validation of the HPLC method applied to the actual drug samples was also performed.
Açıklama
Fen Bilimleri Enstitüsü, Kimya Ana Bilim Dalı
Anahtar Kelimeler
Kimya, Chemistry
