METHOD VALIDATION FOR DETERMINATION OF SILDENAFIL CITRATE IN EXTEMPORANEOUS ORAL SUSPENSION
Keywords:
Sildenafil Citrate, HPLC, Validation, Extemporaneous, SuspensionAbstract
Â
Objective: The aim of this study was to validate a high-performance liquid chromatographic (HPLC) method for analysis of sildenafil citrate in an extemporaneous preparation, according to ASEAN guideline for the validation of analytical procedure.
Methods: The chromatographic condition used a C18 column with a mobile phase consisted of 50% 0.2 M ammonium acetate buffer pH 7.0 and 50% acetonitrile. The flow rate was performed at 1.0 mL/min, and UV detection was monitored at 245 nm.
Results: It was shown that the retention time of sildenafil was about 8.80 min. The analytical method used was specific to sildenafil in the presence of other common excipients in the preparation. The method was accurate (100.18% recovery), precise (< 2% RSD), and robust. Linear correlation was obtained over a concentration range of 0.01 - 60.00 mg/mL (r2 = 0.9999). Limit of detection (LOD) and limit of quantification (LOQ) were 3.82 and 11.57 ng/mL, respectively. Forced degradation showed that the method would serve as a stability-indicating procedure that applied for the analysis of the drug in the stability studies.
Conclusion: The proposed method met the general requirements with an acceptable performance for validation. It was accurate and reliable, and served as a stability-indicating method. Therefore, it can be used to determine sildenafil citrate in the extemporaneous suspension preparation.
Downloads
References
Corbin JD, Francis SH, Cyclic GMP, J. phosphodiesterase-target of sildenafil. J Chem 1999;5(274):13729-32.
Card GL, England BP, Suzuki Y, Fong D, Powell B, Lee B, et al. Structural basis for the activity of drugs that inhibit phosphodiesterases. Structure (London, England:1993). 2004;12(12):2233-47.
Al-Omari MM, Zughul MB, Davies JED, Badwan AA, J. Sildenafil/cyclodextrin complexation:Stability constants, thermodynamics, and guest-host interactions probed by 1H NMR and molecular modeling studies. J Biomed Anal 2006;41:857-65.
Ghofrani HA, Osterloh IH, Grimminger F. Sildenafil:from angina to erectile dysfunction to pulmonary hypertension and beyond. J Nature Reviews Drug Discovery 2006;5(8):689-702.
Huddleston AJ, Knoderer CA, Morris JL, Ebenroth ES. Sildenafil for the treatment of pulmonary hypertension in pediatric patients. J Pediatr Cardiol 2009;30(7):871-82.
Jackson M, Lowey A. editors. Handbook of extemporaneous preparation:A guide to pharmaceutical compounding2010. 363-7
Dinesh ND, Vishukumar BK, Nagaraja P, Made Gowda NM, Rangappa KS. Stability indicating RP-LC determination of sildenafil citrate (Viagra) in pure form and in pharmaceutical samples. J Pharm Biomed Anal 2002;29(4):743-8.
Ahmed NR, Lottfi SN. High performance liquid chromatographic method for determination of sildenafil citrate (Viagra) in pharmaceutical formulation and industrial effluent sample. Raf J Sci 2013;24:24-31.
Reddy BPK, Reddy YR. Validation and stability indicating RP-HPLC method for the determination of sildenafil citrate in pharmaceutical formulations and human plasma. E-J Chem 2008;5 (Suppl 2):1117-22.
Audu SA, Ogunbameru W, Sani MA, Abdulraheem RO, Abdulraheem RB, J. Quantitative determination of sildenafil citrate in commercial tablet dosage form marked in Maidugri Metropolitan Council (MMC). Int Res AAPS Pharm Sci Tech 2012;3:91-3.
Mahmood KT, Khan B, J. A validated HPLC method for the measurement of sildenafil citrate in different formulations. J Pak 2010;62:192-7.
El-Gindy AE, Shokry E, Farouk M, El-Aziz A, J. Validated methods for determination of sildenafil citrate in the presence of its potential impurities. J Sci Res 2010;2:262-78.
Rajyalakshmi CH, Benjamin T, Rambabu C, J. Stability indicating RP-HPLC method for simultaneous determination of sildenafil and duloxetine in pharmaceutical dosage form. J Am Tech Res 2013;3:971-84.
Sawatdee S, Srichana T. Analytical validation of sildenafil citrate inhaler preparation. Chiang Mai J Sci 2013;40:669-80.
Yi E-J, Kim J-Y, Rhee Y-S, Kim S-H, Lee H-J, Park C-W, et al. Preparation of sildenafil citrate microcapsules and in vitro/in vivo evaluation of taste masking efficiency. Int J Pharm 2014;466(1-2):286-95.
Elshafeey AH, Bendas ER, Mohamed OH. Intranasal microemulsion of sildenafil citrate:in vitro evaluation and in vivo pharmacokinetic study in rabbits. J AAPS Pharm Sci Tech 2009;10(2):361-7.
Asean. ASEAN guideline on analytical validation 2004. 1-18
Nahata MC, Morosco RS, Brady MT. Extemporaneous sildenafil citrate oral suspensions for the treatment of pulmonary hypertension in children. American journal of health-system pharmacy:AJHP:official J of the American Society of Health-System Pharmacists 2006;63(3):254-7.
Daraghmeh N, Al-Omari M, Badwan AA, Jaber AM. Determination of sildenafil citrate and related substances in the commercial products and tablet dosage form using HPLC. J Pharm Biomed Anal 2001;25(3-4):483-92.
Garcia JS, Trevisan MG, J. Júlio TA, Zâmara IF, Compatibility of sildenafil citrate and pharmaceutical excipients by thermal analysis and LC-UV. J Anal Calorim 2013;111:2037-44.
Özkan SA, Uslu B, Zuma P. Electrochemical oxidation of sildenafil citrate (Viagra) on carbon electrodes. J Anal Chim Acta 2004;501:227-33.
Lia J, Chang TW. Determination of transdermal sildenafil in nude mouse skin by reversed-phase high-performance liquid chromatography. J of Chromatography B, Biomedical Sci and Appl 2001;765(2):161-6.
Awofisayo OS, Awofisayo OA, Eyen N, Uslu B, J., Zuma P. Development of basic tests for sildenafil citrate and sildenafil citrate tablet. J Med Res 23 zkan SA Electrochemical oxidation of sildenafil citrate Viagra on carbon electrodes. J Anal Chim Acta 50122733. 2004;2:175-9.
Badawy AM, El-Aleem A, Lamie NT, J. Stability indicating methods for the determination of sildenafil citrate in the presence of its degradation product. Int Pharm 2011;7:1-6.
Bakshi M, Singh S. Development of validated stability-indicating assay methods--critical review. J Pharm Biomed Anal 2002;28(6):1011-40.
Mannur VS, Rathi SM, Mastiholimath VS, Dengale NP, Shinde TA, J. Stability indicating RP-HPLC method development and validation of sildenafil citrate in pure form. Int Pharm Sci 2011;2:187-91.