DEVELOPMENT AND VALIDATION OF RP-HPLC AND UV SPECTROPHOTOMETRIC METHODS FOR THE QUANTIFICATION OF CAPECITABINE
Keywords:
Capecitabine, UV spectrophotometric, Forced degradation, RP-HPLC, Method validationAbstract
Objective: The objective of the present study was to develop and validate a new liquid chromatographic technique and four new spectrophotometric methods for the quantitative estimation of Capecitabine.
Methods: In the first method, the chromatographic technique was carried out in isocratic technique on Shimadzu Model CBM-20A/20 Alite HPLC system, equipped with SPD M20A prominence PDA detector with Zorbax C18 (150 mm × 4.6 mm i. d, 5 µm particle size) column. The method was optimized with a mobile phase consisting of 0.1 % Acetic acid and Acetonitrile (35:65, v/v) with flow rate 0.5 ml/min. In second, third, fourth and fifth methods, spectrophotometric techniques were applied. The absorption maximum (λmax) was observed at 305 nm, 305 nm, 303 nm and 297 nm for method B (developed in 0.1 N hydrochloric acid), C (developed in sodium acetate buffer pH 4.0), D (developed in phosphate buffer pH 7.0) and E (developed in borate buffer pH 9.0) respectively. Different validation parameters such as linearity, precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ), robustness were also determined.
Results: The linearity of the calibration curves for the analyte in the desired concentration range is good for both the HPLC (R2 = 0.9994) and UV methods. The LOD and LOQ were found to be 0.02354 μg/ml and 0.07162 μg/ml respectively. The % RSD values for the validation parameters (precision and accuracy) were less than 2.0%.
Conclusion: The proposed chromatographic and spectrophotometric methods were validated and can be applied for the determination of Capecitabine in pharmaceutical formulations.
Keywords: Capecitabine, UV spectrophotometric, ÂÂForced degradation, RP-HPLC, Method validation
Downloads
References
Anonymous. Indian pharmacopoeia. Vol 2. Controller of Publications; Govt. of India; 2010. p. 972-3.
Anonymous. United States of pharmacopeia. Vol 2. The United States of Pharmacopeia-National Formulary; 2008. p. 1620-2.
Katzung BG, Trevor AJ, Masters SB. Basic and clinical pharmacology. 11th ed. McGraw-Hill Medical Publishing Division; 2009. p. 947.
Hardman JG, Limbird LE, Gilman AG. Goodman and gilman’s the pharmacological basis of therapeutics. 10th ed. New York: McGraw-Hill; 2001. p. 1404-5.
Lanjhiyana SK, Dang JS, Garabadu D, Lanjhiyana S, Garabadu PS, Arya A. In vitro drug release studies of 5-fluorouracil from novel enteric coated capsules utilizing combined approaches of pH-dependent and microbial-triggered biodegradable polysaccharides for colon-specific delivery. Der Pharm Lett 2010;2:255-73.
Rao ST, Sukanya K, Sreedhar C, Akkamma HG, Kumar SS, Manogna. Development and validation of new analytical methods for the estimation of capecitabine in pharmaceutical dosage form. Res J Pharm Biol Chem Sci 2012;3:713-21.
Prashanthi D, Raj Kumar B, Nagarajan G, Jona Methusala R, Prasanthi A. A new analytical method development and validation of Capecitabine in pure and tablet dosage forms by UV Spectroscopy. Int J Med Nanotechnol 2014;1:48-53.
Kumbhar SC, Salunkhe VR. UV-Spectrophotometric method development for Capecitabine in eudragit and chitosan based microspheres and its validation. Indian J Pharm Biol Res 2013;1:32-8.
Rao MS, Ramesh G. Development and validation of a simple and specific UV spectrophotometric method for capecitabine assay in active pharmaceutical ingredients (API) and in its dosage forms. Int J Pharm Pharm Res 2015;2:152-60.
Jothieswari D, Reddy CB, Swarna Latha G, Sowkar Baig I, Reddy KB, Dhanalakshmi K. Development and validation Of UV-spectroscopic method for determination of Capecitabine in bulk and formulation. Int J Med Chem Anal 2014;4:279-83.
Kandimalla R, Nagavalli D. Validated estimation of Capecitabine by UV-spectroscopic RP-HPLC and HPTLC method. Int Res J Pharm 2012;3:163-6.
Kumar NM, Sankar PR, Viswanath A, Babu PS. Validated UV spectrophotometric method for quantitative analysis of Capecitabine in pharmaceutical dosage form. J Chem Pharm Sci 2013;6:231-3.
Patel SH, Patel PU. Development and validation of pH independent spectroscopic method for determination of capecitabine. Der Pharm Sinica 2015;6:19-23.
Pani Kumar AD, Raju VY, Sunitha G, Rama Krishna K, Ceema M, Rao VA. Development of validated stability indicating RP-HPLC method for the estimation of capecitabine in pure and pharmaceutical formulations. Int J Res Pharm Biomed Sci 2011;2:175-81.
Jayaseelan S, Bajivali SK, Ramesh U, Sekar V, Perumal P. Bioanalytical method development and validation of Capecitabine by RP-HPLC method. Int J ChemTech Res 2010;2:2086-90.
Sreevatsav ASK, Harishbabu AK. RP-HPLC method development and validation of Capecitabine extended release tablet dosage form. Int J Pharm Sci Res 2013;4:4477-87.
Makula A, Anjum F, Tangadpally R, Kondepudi RK. Analytical method development and validation of Capecitabine in bulk by RP-HPLC method. Int Res J Pharm 2012;3:177-80.
Devanaboyina N, Sai Kishore Y, Pushpalatha P, Mamatha N, Venkatesh P. Development and validation of New RP HPLC method for analysis of Capecitabine in pharmaceutical dosage form. Int J Sci Inventions Today 2013;2:21-30.
Ravisankar P, Rao GD, Kumar MN, Chaitanya MK. An improved RP-HPLC method for the quantitative determination of capecitabine in bulk and pharmaceutical tablet dosage form. Der Pharm Lett 2013;5:249-60.
Karthik A, Vasantha K, Suneetha GL, Sai Sree M, Nalluri BN. Development of validated RP-HPLC-PDA method for the analysis of Capecitabine in bulk, dosage forms and in dissolution samples. J Chem Pharm Res 2014;6:319-25.
Prakash KV, Rao VJ, Raju NA. Validated reversed phase high-performance liquid chromatography method for the estimation of Capecitabine in pharmaceutical formulations. Orient J Chem 2008;24:335-8.
Edla S, Sundhar BS. A novel RP-HPLC method for the determination of Capecitabine in pharmaceutical drug products. Res Desk 2012;1:10-7.
Kishore M, Jayaprakash M, Reddy TVB. Spectrophotometric determination of capecitabine in pharmaceutical formulations. Int J ChemTech Res 2011;3:63-9.
Siethoff C, Orth M, Ortling A, Brendel E, Wagner-Redeker W. Simultaneous determination of Capecitabine and its metabolite 5-fluorouracil by column switching and liquid chromatographic/tandem mass spectrometry. J Mass Spectrom 2004;39:884–9.
Anonymous. International Conference on Harmonization (ICH). Q2 (R1), Text on Validation of Analytical Procedures, Geneva, Switzerland; 2005.