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Quantification of solid-state impurity with powder X-ray diffraction using laboratory source

Published online by Cambridge University Press:  27 July 2020

Meenakshi Sundaram ,
Saravanan Natarajan ,
Amol G. Dikundwar Open the ORCID record for Amol G. Dikundwar [Opens in a new window]  and
Hemant Bhutani Open the ORCID record for Hemant Bhutani [Opens in a new window]
Meenakshi Sundaram
Affiliation:
Analytical R&D, Pharmaceutical Development, Biocon Bristol-Myers Squibb Research and Development Center, Syngene International Limited, Bangalore560099, India
Saravanan Natarajan
Affiliation:
Analytical R&D, Pharmaceutical Development, Biocon Bristol-Myers Squibb Research and Development Center, Syngene International Limited, Bangalore560099, India
Amol G. Dikundwar*
Affiliation:
Analytical R&D, Pharmaceutical Development, Biocon Bristol-Myers Squibb Research and Development Center, Syngene International Limited, Bangalore560099, India
Hemant Bhutani*
Affiliation:
Analytical R&D, Pharmaceutical Development, Biocon Bristol-Myers Squibb Research and Development Center, Bristol-Myers Squibb India Private Limited, Bangalore560099, India
*
a)Authors to whom correspondence should be addressed. Electronic mail: amoldiku@gmail.com (A. G. D.); hemant.bhutani@bms.com (H. B.)
a)Authors to whom correspondence should be addressed. Electronic mail: amoldiku@gmail.com (A. G. D.); hemant.bhutani@bms.com (H. B.)
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Abstract

The application of powder X-ray diffraction (PXRD) for the detection and quantification of low levels of a solid-state chemical impurity, BrettPhos oxide, in an active pharmaceutical ingredient is discussed. It is demonstrated that with appropriate methodology and experimentation, the impurity levels of as low as 0.07% w/w could be detected reliably and limit of quantification of 0.10% w/w could be achieved by PXRD, using a laboratory X-ray source. Method development, validation, and benchmarking using conventional high-performance liquid chromatography are presented in the manuscript highlighting the robustness and reproducibility of such measurements.

Keywords

powder X-ray diffractionquantitative analysisHPLCBrettPhos oxidesingle peak analysiscrystalline impurity
Type
Technical Article
Information
Powder Diffraction , Volume 35 , Issue 4 , December 2020 , pp. 226 - 232
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Copyright
Copyright © 2020 International Centre for Diffraction Data

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