Ters Faz Sıvı Kromatografi Yöntemiyle İlaç Formülasyonunda Pravastatin Tayini İçin Geliştirilmiş Optimizasyon Çalışması

Yıl 2017, Cilt: 7 Sayı: 2, 602 - 607, 01.06.2017

Zehra Üstün Yaşar Doğan Daldal Aybike Talay Ebru Çubuk Demiralay

Öz

Pravastatin, anti-kolesterol ajanlar grubuna dahil olan ve yüksek kolesterol tedavisinde kullanılan bir ilaçtır. Bu çalışmada pravastatinin tablet formulasyonundan tayini için ters faz sıvı kromatografi RPLC metodu tanımlanmıştır. Önerilen metot mobil faz pH’sında küçük değişiklik yapılarak geliştirilmiştir. Kromatografik ayrım C18 kolon kullanılarak, asetonitril-su 40:60, v/v ikili mobil faz karışımında gerçekleştirilmiştir. Akış hızının 1 mL/dakika olduğu çalışma 239 nm’de yürütülmüştür. Çalışmada lineer aralık 2-12 μg/mL olarak belirlenmiştir. Pravastatin için dedeksiyon limiti LOD ve kantitatif yorum limiti LOQ değerleri sırasıyla 0.260 μg/mL ve 0.787 μg/mL olarak olarak ölçülmüştür. Optimizasyon sonuçları, istatistiksel verilerle birlikte değerlendirildiğinde metodun güvenilirliğini ortaya koymaktadır

Anahtar Kelimeler

Anti-kolesterol ajanlar, Farmasötik dozaj form, RPLC, UV dedeksiyon

An Improved Optimization Study for Determination of Pravastatin in Pharmaceutical Form by using Reversed Phase Liquid Chromatography Method

Öz

Pravastatin belongs to the group of anticholestrol agents used in the treatment of hypercholestaraemia. Reversed phase liquid chromatographic RPLC method was described in this study for its determination from tablet formulation. This method was improved with a slight change in the pH of the mobile phase. The experiment was carried out a C18 column with a mobile phase of a binary mixture of acetonitrile and water 40:60, v/v delivered at a flow rate of 1 mL/min and detection was carried out at 239 nm. The linear range was found as 2 - 12 μg/mL. The lower of quantitation LOQ for pravastatin was 0.787 µg/mL. The optimization results, together with statistical evaluation of the data, demonstrated the reliability of this method.

Anahtar Kelimeler

Anticholestrol agents, Reversed Phase Liquid Chromatography RPLC, UV detection, Pharmaceutical dosage form

Kaynakça

• Hatanaka, T. 2000. Clinical pharmacokinetics of pravastatin. Clin. Pharm., 39(6): 397-412.
• Quion, JA., Jones, PH. 1994. Clinical pharmacokinetics of pravastatin. Clin. Pharm., 27(2): 94-103.
• Jungnickel, PW., Cantral, KA., Maloley, PA. 1992. Pravastatin: a new drug for the treatment of hypercholesterolemia. Clin. Pharmacy, 11(8): 677-689.
• Gomes, FP., Garcia, PL., Alves, JMP., Singh, .K., KedorHackmann, ERM., Santoro, MIRM. 2009. Development and validation of stability-indicating HPLC methods for quantitative determination of pravastatin, fluvastatin, atorvastatin and rosuvastatin in pharmaceuticals. Anal. Lett., 42(12): 1784-1804.
• Chaudhari, BG., Patel, NM., Shah, PB. 2007. Determination of simvastatin, pravastatin sodium and rosuvastatin calcium in tablet dosage forms by HPTLC. Indian J of Pharm Sci, 69(1): 130-132.
• Campos-Lara, M., Mendoza-Espinoza, JA. 2008. Development of a selective extraction method for pravastatin quantification in tablets using HPLC with ultraviolet detection. J Liq Chromatogr Relat Technol, 31(4): 619-623.
• Önal, A., Sagirli, O. 2006. Development of a selective LC method for determination of pravastatin sodium. Chromatographia, 64(3-4): 1-6.
• Ashour, S., Nakshbandi, H., Omar, S. 2008. Quantitave determination of pravastatin in pharmaceutical dosage forms by High-Performance Liquid Chromatography with ultraviolet detection. Int J Biomed Sci, 4(2): 135-139.
• Sultana, N., Arayne, MS., Shaazad, W. 2010. Simultaneous determination os ceftriaxone sodium and statin drugs in pharmaceutical formulations and human serum by RP-HPLC. J Chil Chem Soc, 55(2): 193-198.
• Smith, C., Khaledi, MG. 1993. Optimization of pH for the separation of organic acids in capillary zone electrophoresis. Anal Chem, 65(3): 193-198.
• Rosés, M., Canals, I., Allemann, H., Siigur, K., Bosch, E. 1996. Retention of ionizable compounds on hplc. 2. effect of ph, ıonic strength, and mobile phase composition on the retention of weak acids. Anal Chem, 68: 4094-4100.
• Talay, A., Demiralay, EÇ., Daldal, YD., Üstün, Z. 2015. Investigation of thermodynamic acidity constants of some statins with RPLC method. J Mol Liq, 208(38): 286-290.
• Rondinini, S., Mussini, PR., Mussini, T. 1987. Reference value standards and primary standards for pH measurements in organic solvents and water+organic solvent mixtures of moderate to high permittivities. Pure App Chem, 59:1549- 1560.
• NLREG Version 4.0. P.H. Sherrod, http://www.sandh.com/ Sherrod1991
• McNally, R. 2000. The United States Pharmacopoeia, 24th revision, Q5 Taunton, M.A.