Research Journal of Pharmacy and Technology

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Development and Validation of an Analytical Liquid Chromatography-Tandem Mass Spectroscopy Method for the Estimation Febuxostat in Pharmaceutical Formulation


Affiliations
1 Department of Pharmaceutical Analysis, JSS College of Pharmacy (JSS Academy of Higher Education and Research, Mysuru) Udhagamandalam, India
2 Indian Pharmacopoeia Commission, New Delhi, India
     

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A rapid LC-MS/MS method has been developed and validated for the quantitative determination of Febuxostat from the commercially available formulations. The separation was achieved using Zorbax SB C18 column (4.6 × 50 mm, 5 μm) as a stationary phase and the mobile phase consists of (10 mM) Ammonium formate (pH4.0): methanol (10:90 v/v) with a flow of 0.6 mL/min. Detection was carried out by triple quadrupole mass spectrometry with electrospray ionization in positive mode with proton adducts at m/z 316.95→260.95 to monitor Febuxostat within a run time of 2 min. The linearity of the method was found over a concentration range of 4 to 55 ng/mL with a regression analysis of 0.997. The percentage recovery of the present method was found to be 97.16 to 99.46%. The LC-MS/MS method was validated as per ICH guidelines. The developed method can be successfully applied for the estimation of Febuxostat in the commercial formulation and in bulk drug.

Keywords

Febuxostat, Formulation, LC-MS/MS, Validation, Electrospray Ionization.
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  • Drug details, URL: https://pubchem.ncbi.nlm.nih.gov/compound/Febuxostat#section=Top

  • Rajyalakshmi Ch., Benjamin T., Ram Babu C. Development and Validation of Zero and First Order Derivative UV-Spectrophotometric Method for Determination of Febuxostat in Bulk and in Formulation. Research. J. Pharm. and Tech. 2013; 6(2): 208-211.

  • J. M. Derasari, V. B. Patel. Spectrophotometric Determination of Febuxostat and Diclofenac Potassium in Their Combined Dosage Form by Simultaneous Equation and First Order Derivative Methods. Asian J. Research Chem. 2013; 6(10): Page 968-972.

  • D. M. Darandale, K.B. Erande, S.R. Tambe, R.S. Bhamber. Development and Validation of RP-HPLC Method for the Determination of Febuxostat in Bulk and Pharmaceutical Dosage Form. Asian J. Research Chem. 2017; 10(6):713-718.

  • Muvvala SS, Ratnakaram VN, Nadendla RR. Validated RP-HPLC method for the estimation of febuxostat in bulk drugs. Int J pharmTech Res. 2012; 4(4): 1358-1366.

  • Kumar RS, Ravikumar BVV, Anjaya Kumar P. A RP-HPLC method development and validation for estimation of febuxostat bulk and pharmaceutical dosage forms. Int Res J Pharm. 2012; 3(11): 205-208.

  • Chandu BR, Kanala K, Hwisa NT, Katakam P, Khagga M. Bio-equivalance and pharmacokinetic study of febuxostat in human plasma by using LC-MS/MS with liquid liquid extraction method. Spinger plus, 2013; 2(194): 1-10.

  • Pal N, Rao AS, Kumar PR. New method development and validation for the determination of febuxostat in human plasma by liquid chromatography –mass spectrometry. Int J Pharm Pharm Sci. 2016; 8(9): 61-70.

  • Mitesh D Phale, Dipti Korgaonkar. Current Advance Analytical Techniques: A Review. Asian J. Research Chem. 2009; 2(3): 235-238.

  • ICH validation, URL:https://www.ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines/Quality/Q2_R1/Step4/Q2_R1__Guideline.pdf.


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  • Development and Validation of an Analytical Liquid Chromatography-Tandem Mass Spectroscopy Method for the Estimation Febuxostat in Pharmaceutical Formulation

Abstract Views: 268  |  PDF Views: 0

Authors

Lingamallu Venkata Sai Krishna
Department of Pharmaceutical Analysis, JSS College of Pharmacy (JSS Academy of Higher Education and Research, Mysuru) Udhagamandalam, India
S. T. Narenderan
Department of Pharmaceutical Analysis, JSS College of Pharmacy (JSS Academy of Higher Education and Research, Mysuru) Udhagamandalam, India
Ramshankar Nayak
Department of Pharmaceutical Analysis, JSS College of Pharmacy (JSS Academy of Higher Education and Research, Mysuru) Udhagamandalam, India
S. N. Meyyanathan
Department of Pharmaceutical Analysis, JSS College of Pharmacy (JSS Academy of Higher Education and Research, Mysuru) Udhagamandalam, India
B. Babu
Department of Pharmaceutical Analysis, JSS College of Pharmacy (JSS Academy of Higher Education and Research, Mysuru) Udhagamandalam, India
M. Kalaivani
Indian Pharmacopoeia Commission, New Delhi, India

Abstract


A rapid LC-MS/MS method has been developed and validated for the quantitative determination of Febuxostat from the commercially available formulations. The separation was achieved using Zorbax SB C18 column (4.6 × 50 mm, 5 μm) as a stationary phase and the mobile phase consists of (10 mM) Ammonium formate (pH4.0): methanol (10:90 v/v) with a flow of 0.6 mL/min. Detection was carried out by triple quadrupole mass spectrometry with electrospray ionization in positive mode with proton adducts at m/z 316.95→260.95 to monitor Febuxostat within a run time of 2 min. The linearity of the method was found over a concentration range of 4 to 55 ng/mL with a regression analysis of 0.997. The percentage recovery of the present method was found to be 97.16 to 99.46%. The LC-MS/MS method was validated as per ICH guidelines. The developed method can be successfully applied for the estimation of Febuxostat in the commercial formulation and in bulk drug.

Keywords


Febuxostat, Formulation, LC-MS/MS, Validation, Electrospray Ionization.

References