In the pharmaceutical industry, the unexpected appearance of crystalline forms could impact the therapeutic efficacy of an Active Pharmaceutical Ingredient (API). For quality control, a thorough qualitative and quantitative monitoring of pharmaceutical solid forms is essential to ensure the detection and the quantification of crystalline forms, wither different or with the same chemical composition (polymorphs) at a low detection level. The purpose of this paper was to review and highlight the importance of choosing adequate solid-state techniques for detection and quantification APIs that present polymorphism - based on limits of detection (LOD) and quantification (LOQ), pharmacopeias specifications, international guidelines and studies reported in the literature. To this study, the powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), Infrared and Raman spectroscopies and solid-state nuclear magnetic resonance (NMR) were the solid-state techniques analyzed. Additionally, the Argentine, Brazilian, British, European, International, Japanese, Mexican and the United States of America pharmacopeias were reviewed. Based on the analysis performed, the advantages and disadvantages of these techniques, as well as the LOD and LOQ values of APIs were reported. In comparison to these solid-state techniques, reference material used for identification analyses should be previously identified with the corresponding polymorph. Without this previous procedure, the patterns, the spectra, and DSC curves of the reference material can only be used to confirm the mixture of solid forms, not being able to specify which polymorphs are contained in the sample. A major advantage of PXRD is the use of the calculated diffraction patterns obtained from the Crystallographic Information Frameworks (CIFs) files which could be used as a reference pattern without any other information, assistance technique, or physical standards. Regarding the quantification aspect, different pharmacopeias suggest various methods such as the PXRD combining with Rietveld method, which can be used to obtain lower LOD values for minority phases in the mixture of different substances without the need for a calibration curve. Raman spectroscopy can detect polymorphs in small particles and solid-state NMR spectroscopy is a powerful technique for quantification not only crystalline but also crystalline-amorphous mixtures. Finally, this review intends to be a useful tool to control, with efficiency and accuracy, the polymorphism of APIs in pharmaceutical compounds.

Over the past decades Raman spectroscopy has been extensively used both on an industrial and academic level. This has resulted in the development of numerous specialized Raman techniques and Raman active products, which in turn has led to the adoption and development of standards and norms pertaining to Raman unit\'s calibration, performance validation, and interoperability. Purpose of the present review is to list, classify, and engage in a comprehensive analysis of the different standards, guides, and practices relating to Raman spectroscopy. Primary aim of the review is to consider the commonalities and conflicts between these standards and norms and to identify any missing aspects. Standardization in the field of Raman spectroscopy is dominated by the work of American institutions, namely, the American Society of Testing Materials (ASTM or ASTM International), with several active standards in place pertaining to terminology, calibration, multivariate analysis, and specific applications, and the National Institute of Standards and Technology (NIST), providing numerous certified reference materials, referred to as standard reference materials. The industrial application of Raman spectroscopy is dominated by the pharmaceutical industry. As such, pharmacopoeias provide not only important information in relation to pharmaceutical-related applications of Raman spectroscopy, but also invaluable insight, into the basic principles of Raman spectroscopy and important aspects that include calibration, validation, measurement, and chemometric analysis processes, usually by referring to ASTM and NIST standards. Given the fact that Raman spectroscopy is a modern and innovative field, the standardization processes are complex and constantly evolving. Despite the seemingly high number of existing standards, the standardization landscape is incomplete and has not been modernized according to the developments in Raman spectroscopy techniques in recent years. This is evident by the lack of protocols for numerous areas as well as by the fact that some of the existing standards have not been updated to reflect the advances in the technique. Therefore, it is important for the Raman community to actively engage in and contribute to a modernization process that will result in updating existing and introducing new terms, protocols, and guides. Indeed, the development of optimized common standards would be extremely beneficial and would further foster the development and application of Raman spectroscopy techniques, most notably those of surface enhanced Raman spectroscopy and low-resolution portable analyzers.

暂无摘要。

暂无摘要。

暂无摘要。

暂无摘要。

暂无摘要。