Citation: Zhao Yu-Mei, Zheng Zhi-Bing, Li Song. Quantification of flupirtine maleate polymorphs using X-ray powder diffraction[J]. Chinese Chemical Letters, ;2016, 27(11): 1666-1672. doi: 10.1016/j.cclet.2016.03.042 shu

Quantification of flupirtine maleate polymorphs using X-ray powder diffraction

Zhao Yu-Mei ^a,b ,
Zheng Zhi-Bing ^a,, ,
Li Song ^a,c,,

a.
Laboratory of Computer-Aided Drug Design & Discovery, Beijing Institute of Pharmacology and Toxicology, Beijing 100850, China
b.
Laboratory of Structure Identification, Beijing Institute of Pharmacology and Toxicology, Beijing 100850, China
c.
State Key Laboratory of Toxicology and Medical Countermeasures, Beijing Institute of Pharmacology and Toxicology, Beijing 100850, China

Corresponding author: Zheng Zhi-Bing, zzbcaptain@aliyun.com Li Song, lis@nic.bmi.ac.cn
Received Date: 18 February 2016
Revised Date: 14 March 2016
Accepted Date: 17 March 2016
Available Online: 11 November 2016

Figures(10)

Flupirtine maleate, a pharmaceutical compound for treating psychotic disease in clinics, has seven polymorphs.Form A, with better crystal stability and bioavailability, has been widely used as the pharmaceutical crystal form.Unfortunately, it is usually found in a polymorphic mixture with form B.In this study, pure crystal forms of A and B were prepared and characterized by X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FT-IR) and thermal analysis.An XRPD-based method for the quantitative determination of the amount of the flupirtine maleate polymorphs form A and form B was also established through a systematic optimization of instrumental parameters.The results of the analytical methodology validation showed that the XPRD method had a broad quantitative range of 0-100%(w/w), good linear relationship, with R²=0.999, excellent repeatability and precision and low limits of detection (LoD) of 0.15%(w/w) and quantification (LoQ) of 0.5%(w/w).The results also showed that the single-peak method was not as good as the whole pattern in reducing the influence of the preferred orientation, but this can be compensated for by a systematic optimization of instrumental parameters and validating the analytical methodology to reduce errors and obtain a good, repeatable, sensitive, and accurate method.This XRPD method can be used to analyze mixtures of flupirtine maleate polymorphs (forms A and B) quantitatively and control the quality of the bulk drug.
- Flupirtine maleate,
- X-ray powder diffraction,
- Quantitative analysis of polymorphs,
- Preferred orientation,
- Transmission
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