Quantifying API polymorphs in formulations using X-ray powder diffraction and multivariate standard addition method combined with net analyte signal analysis

Zappi, Alessandro; Maini, Lucia; Galimberti, Giuliano; Caliandro, Rocco; Melucci, Dora

doi:10.1016/j.ejps.2019.01.014

Cited by 15 publications

(2 citation statements)

References 34 publications

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“…Quantitative analysis of the weight amount of an individual crystal phase in a complex mixture of unknown composition can be challenging. In the work of Zappi et al (2019), the quantification of the active pharmaceutical compound (API) paracetamol (polymorphic form I) in a solid formulation of the commercial drug Tachifludec was considered as a case study. In the first instance, the commercial sample was measured by PXRD in three replicates and the known crystal phase was analysed using the MultiFit procedure of RootProf, as shown in Fig.…”

Section: Quantitative Analysismentioning

confidence: 99%

New features of the RootProf program for model-free analysis of unidimensional profiles

Mazzone,

Lopresti,

Belviso

et al. 2023

J Appl Crystallogr

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The RootProf computer program applies multivariate model-free analysis to crystallographic data and to any x, y experimental data in general. It has been enhanced with several new features, including a graphical user interface, multithreading implementation and additional pre-processing options. The program also includes novel qualitative analysis methods, such as semiquantitative estimates derived from principal component analysis (PCA) and restrained PCA to extract the diffraction signal from active atoms. Additional quantitative analysis methods have been included, involving the combination of different datasets or the application of the standard addition method as well as tools for crystallinity analysis, kinetic analysis and extraction of free crystal cell parameters from a pair distribution function profile. The ROOT data analysis framework supports the program and can be installed on the current major platforms such as Windows, Linux and Mac OSX with detailed user documentation included. Applications of the new developments are presented and discussed in the paper, and related command files are provided as supporting information.

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Section: Quantitative Analysismentioning

confidence: 99%

New features of the RootProf program for model-free analysis of unidimensional profiles

Mazzone,

Lopresti,

Belviso

et al. 2023

J Appl Crystallogr

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“…to exploit RR. Multivariate statistical analysis (MSA), requiring no or little a priori information, is a recently explored alternative (Caliandro et al, 2013;Zappi et al, 2019;Guccione et al, 2021) to the above-cited traditional approaches (widely described in Appendix A) of XRPD and XRF data analysis. The MultiFit regression procedure (Caliandro & Belviso, 2014) requires only pure phase profiles, while principal component analysis (PCA) is a completely blind approach (Jolliffe & Cadima, 2016); both approaches, available within RootProf (Caliandro & Belviso, 2014), a software (free for academic use) built specifically to manage XY profiles such as XRPD, XRF or other typical instrumental data, are the topic of the present contribution.…”

Section: Introductionmentioning

confidence: 99%

Multivariate versus traditional quantitative phase analysis of X-ray powder diffraction and fluorescence data of mixtures showing preferred orientation and microabsorption

Lopresti¹,

Mangolini²,

Milanesio³

et al. 2022

J Appl Crystallogr

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In materials and earth science, but also in chemistry, pharmaceutics and engineering, the quantification of elements and crystal phases in solid samples is often essential for a full characterization of materials. The most frequently used techniques for this purpose are X-ray fluorescence (XRF) for elemental analysis and X-ray powder diffraction (XRPD) for phase analysis. In both methods, relations between signal and quantity do exist but they are expressed in terms of complex equations including many parameters related to both sample and instruments, and the dependence on the active element or phase amounts to be determined is convoluted among those parameters. Often real-life samples hold relations not suitable for a direct quantification and, therefore, estimations based only on the values of the relative intensities are affected by large errors. Preferred orientation (PO) and microabsorption (MA) in XRPD cannot usually be avoided, and traditional corrections in Rietveld refinement, such as the Brindley MA correction, are not able, in general, to restore the correct phase quantification. In this work, a multivariate approach, where principal component analysis is exploited alone or combined with regression methods, is used on XRPD profiles collected on ad hoc designed mixtures to face and overcome the typical problems of traditional approaches. Moreover, the partial or no known crystal structure (PONKCS) method was tested on XRPD data, as an example of a hybrid approach between Rietveld and multivariate approaches, to correct for the MA effect. Particular attention is given to the comparison and selection of both method and pre-process, the two key steps for good performance when applying multivariate methods to obtain reliable quantitative estimations from XRPD data, especially when MA and PO are present. A similar approach was tested on XRF data to deal with matrix effects and compared with the more classical fundamental-parameter approach. Finally, useful indications to overcome the difficulties of the general user in managing the parameters for a successful application of multivariate approaches for XRPD and XRF data analysis are given.

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Characterization Tools for Current Drug Delivery Systems

Bhatia,

Malik,

Sampathi

2024

Biosystems, Biomedical &Amp; Drug Delivery Systems

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Quantifying API polymorphs in formulations using X-ray powder diffraction and multivariate standard addition method combined with net analyte signal analysis

Cited by 15 publications

References 34 publications

New features of the RootProf program for model-free analysis of unidimensional profiles

New features of the RootProf program for model-free analysis of unidimensional profiles

Multivariate versus traditional quantitative phase analysis of X-ray powder diffraction and fluorescence data of mixtures showing preferred orientation and microabsorption

Characterization Tools for Current Drug Delivery Systems

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