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Development of a highly sensitive method for quantitative estimation of Hexamine impurity in Febuxostat drug substances using LC-MS
Abstract
A selective and highly sensitive liquid chromatography-mass spectrometry (LC-MS) method was developed for the determination of Hexamine impurity in Febuxostat drug substance. The method was validated as per International Council for Harmonisation (ICH) guidelines, for which limit of detection and limit of quantitation obtained were 0.75 ppm and 2.26 ppm respectively. The regression coefficient found for the linearity study was 0.9984. The % recovery of the spiked hexamine in drug substance obtained was in the range of 81.9 to 110.5 ensured the accuracy of the method. The method can be adapted to determine hexamine in Febuxostat drug substance (API).
References
Bruce SP. Febuxostat: a selective xanthine oxidase inhibitor for the treatment of hyperuricemia and gout. Annals of Pharmacotherapy. 2006 Dec; 40(12):2187-94.
EFSA Panel on Additives and Products or Substances used in Animal Feed (FEEDAP). Scientific Opinion on the safety and efficacy of hexamethylenetetramine as a silage additive for pigs, poultry, bovines, sheep, goats, rabbits and horses. EFSA Journal. 2015 Feb; 13(2):4014.
Guideline, ICH Harmonized Tripartite. Assessment and Control of DNA Reactive (Mutagenic) Impurities in Pharmaceuticals to Limit Potential Carcinogenic RISK M7. International conference on harmonization of technical requirements for registration of pharmaceuticals for human use (ICH): Geneva. 2014.
Snodin DJ, McCrossen SD. Guidelines and pharmacopoeial standards for pharmaceutical impurities: overview and critical assessment. Regulatory Toxicology and Pharmacology. 2012 Jul 1; 63(2):298-312.
Pavitrapok C, Williams DA. Determination of methenamine, methenamine mandelate and methenamine hippurate in pharmaceutical preparations using ion-exchange HPLC. Journal of pharmaceutical and biomedical analysis. 2006 Mar 18; 40(5):1243-8.
Gautier T, Schmitz-Afonso I, Touboul D, Szopa C, Buch A, Carrasco N. Development of HPLC-Orbitrap method for identification of N-bearing molecules in complex organic material relevant to planetary environments. Icarus. 2016 Sep 1; 275:259-66.
Bouchereau A, Guénot P, Larher F. Analysis of amines in plant materials. Journal of Chromatography B: Biomedical Sciences and Applications. 2000 Sep 29; 747(1-2):49-67.
Lim H, Kim J, Ko K, Kim M. Determination of hexamethylenetetramine in foods by high-performance liquid chromatography (HPLC). Food Additives & Contaminants: Part A. 2014 Sep 2; 31(9):1489-95.
Balasubramanian M, Thennarasu S, Sudhakaran T, Perumal PT. Spectrophotometric and fluorimetric determination of hexamine in pure form and its pharmaceutical formulation. Biological and Pharmaceutical Bulletin. 2003; 26(8):1211-4.
Castillo M, Barcelo D, Pereira AS, Neto FA. Characterization of organic pollutants in industrial effluents by high-temperature gas chromatography-mass spectrometry. TrAC Trends in Analytical Chemistry. 1999 Jan 1; 18(1):26-36.
Paseiro‐Cerrato R, De Quirós AR, Sendón R, Bustos J, Santillana MI, Cruz JM, Paseiro‐Losada P. Chromatographic Methods for the Determination of Polyfunctional Amines and Related Compounds Used as Monomers and Additives in Food Packaging Materials: A State‐of‐the‐Art Review. Comprehensive Reviews in Food Science and Food Safety. 2010 Nov; 9(6):676-94.
Swartz ME, Krull IS. Handbook of analytical validation. CRC Press; 2012 Apr 24.
Chan CC, Lee YC, Lam H, Zhang XM, editors. Analytical method validation and instrument performance verification. John Wiley & Sons; 2004 Apr 23.
Guideline IH. Validation of analytical procedures: text and methodology Q2 (R1). International conference on harmonization, Geneva, Switzerland 2005 Nov (pp. 11-12).
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