title: Quantification of febuxostat polymorphs using powder X-ray diffraction technique.
abstract: Febuxostat is a pharmaceutical compound with more than 20 polymorphs of which form A is most widely used and usually exists in a mixed polymorphic form with form G. In the present study, a quantification method for polymorphic form A and form G of febuxostat (FEB) has been developed using powder X-ray diffraction (PXRD). Prior to development of a quantification method, pure polymorphic form A and form G are characterized. A continuous scan with a scan rate of 3° min(-1) over an angular range of 3-40° 2θ is applied for the construction of the calibration curve using the characteristic peaks of form A at 12.78° 2θ (I/I0100%) and form G at 11.72° 2θ (I/I0100%). The linear regression analysis data for the calibration plots shows good linear relationship with R(2)=0.9985 with respect to peak area in the concentration range 10-60 wt.%. The method is validated for precision, recovery and ruggedness. The limits of detection and quantitation are 1.5% and 4.6%, respectively. The obtained results prove that the method is repeatable, sensitive and accurate. The proposed developed PXRD method can be applied for the quantitative analysis of mixtures of febuxostat polymorphs (forms A and G).
authors: Testing & Analysis Center, Nanjing Normal University, No. 1, Wenyuan Road, Qixia District, Nanjing 210023, Jiangsu Province, PR China.
authors: Jing-bo
authors: JB
authors: Qiu
authors: Testing & Analysis Center, Nanjing Normal University, No. 1, Wenyuan Road, Qixia District, Nanjing 210023, Jiangsu Province, PR China. Electronic address: ligang1@njnu.edu.cn.
authors: Gang
authors: G
authors: Li
authors: Testing & Analysis Center, Nanjing Normal University, No. 1, Wenyuan Road, Qixia District, Nanjing 210023, Jiangsu Province, PR China.
authors: Yue
authors: Y
authors: Sheng
authors: Testing & Analysis Center, Nanjing Normal University, No. 1, Wenyuan Road, Qixia District, Nanjing 210023, Jiangsu Province, PR China.
authors: Mu-rong
authors: MR
authors: Zhu
mesh_terms: D002138:Calibration; D002152:Calorimetry, Differential Scanning / Q000379:methods; D000069465:Febuxostat; D033362:Powder Diffraction / Q000379:methods; D013844:Thiazoles / Q000737:chemistry*; D014961:X-Ray Diffraction / Q000379:methods
chemical_list: D013844:Thiazoles; D000069465:Febuxostat
keywords: Calibration curve; Febuxostat; Polymorph; Powder X-ray diffraction; Quantitative analysis