Yeakub Zaker, Huzeyfe Yilmaz, Timothy R. Lex, Changning Guo, Jason D. Rodriguez, Daniel R. Willett
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In this study, in-house prepared and commercially available tablets were analyzed using LDIR imaging to assess the effects of method development options, particularly the relationship between step size and data acquisition time. Hyperspectral reflectance mode LDIR images were also collected and compared with those obtained from Raman microscopy to validate the accuracy of the LDIR images. The findings emphasize the need for careful wavenumber selection during method development. LDIR images for the evaluated tablets showed good agreement with Raman mapping and hyperspectral mode data sets, although the mean Feret diameter of particles was consistently smaller (14–40 % for active pharmaceutical ingredients (APIs) in the tested tablets) in the LDIR images. Overall, LDIR demonstrates strong potential as a valuable spectroscopic imaging technology for pharmaceutical applications.</div></div>","PeriodicalId":16685,"journal":{"name":"Journal of pharmaceutical and biomedical analysis","volume":"262 ","pages":"Article 116897"},"PeriodicalIF":3.1000,"publicationDate":"2025-04-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Advancing pharmaceutical tablet analysis with laser direct infrared (LDIR) imaging\",\"authors\":\"Yeakub Zaker, Huzeyfe Yilmaz, Timothy R. Lex, Changning Guo, Jason D. Rodriguez, Daniel R. Willett\",\"doi\":\"10.1016/j.jpba.2025.116897\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><div>Laser direct infrared spectroscopy (LDIR) imaging is an emerging vibrational spectroscopic technique that enables rapid surface imaging by using reflectance spectra to capture critical physicochemical properties, such as chemical identity, particle size, shape, and distribution of components, within minutes or even seconds. Despite its advantages, LDIR imaging technology is still in its developmental stages, particularly in understanding method parameters such as the selection of wavenumber for peak and baseline points and the appropriate step size (pixels) for pharmaceutical analysis. In this study, in-house prepared and commercially available tablets were analyzed using LDIR imaging to assess the effects of method development options, particularly the relationship between step size and data acquisition time. Hyperspectral reflectance mode LDIR images were also collected and compared with those obtained from Raman microscopy to validate the accuracy of the LDIR images. The findings emphasize the need for careful wavenumber selection during method development. LDIR images for the evaluated tablets showed good agreement with Raman mapping and hyperspectral mode data sets, although the mean Feret diameter of particles was consistently smaller (14–40 % for active pharmaceutical ingredients (APIs) in the tested tablets) in the LDIR images. Overall, LDIR demonstrates strong potential as a valuable spectroscopic imaging technology for pharmaceutical applications.</div></div>\",\"PeriodicalId\":16685,\"journal\":{\"name\":\"Journal of pharmaceutical and biomedical analysis\",\"volume\":\"262 \",\"pages\":\"Article 116897\"},\"PeriodicalIF\":3.1000,\"publicationDate\":\"2025-04-11\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of pharmaceutical and biomedical analysis\",\"FirstCategoryId\":\"3\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0731708525002389\",\"RegionNum\":3,\"RegionCategory\":\"医学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of pharmaceutical and biomedical analysis","FirstCategoryId":"3","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0731708525002389","RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
Advancing pharmaceutical tablet analysis with laser direct infrared (LDIR) imaging
Laser direct infrared spectroscopy (LDIR) imaging is an emerging vibrational spectroscopic technique that enables rapid surface imaging by using reflectance spectra to capture critical physicochemical properties, such as chemical identity, particle size, shape, and distribution of components, within minutes or even seconds. Despite its advantages, LDIR imaging technology is still in its developmental stages, particularly in understanding method parameters such as the selection of wavenumber for peak and baseline points and the appropriate step size (pixels) for pharmaceutical analysis. In this study, in-house prepared and commercially available tablets were analyzed using LDIR imaging to assess the effects of method development options, particularly the relationship between step size and data acquisition time. Hyperspectral reflectance mode LDIR images were also collected and compared with those obtained from Raman microscopy to validate the accuracy of the LDIR images. The findings emphasize the need for careful wavenumber selection during method development. LDIR images for the evaluated tablets showed good agreement with Raman mapping and hyperspectral mode data sets, although the mean Feret diameter of particles was consistently smaller (14–40 % for active pharmaceutical ingredients (APIs) in the tested tablets) in the LDIR images. Overall, LDIR demonstrates strong potential as a valuable spectroscopic imaging technology for pharmaceutical applications.
期刊介绍:
This journal is an international medium directed towards the needs of academic, clinical, government and industrial analysis by publishing original research reports and critical reviews on pharmaceutical and biomedical analysis. It covers the interdisciplinary aspects of analysis in the pharmaceutical, biomedical and clinical sciences, including developments in analytical methodology, instrumentation, computation and interpretation. Submissions on novel applications focusing on drug purity and stability studies, pharmacokinetics, therapeutic monitoring, metabolic profiling; drug-related aspects of analytical biochemistry and forensic toxicology; quality assurance in the pharmaceutical industry are also welcome.
Studies from areas of well established and poorly selective methods, such as UV-VIS spectrophotometry (including derivative and multi-wavelength measurements), basic electroanalytical (potentiometric, polarographic and voltammetric) methods, fluorimetry, flow-injection analysis, etc. are accepted for publication in exceptional cases only, if a unique and substantial advantage over presently known systems is demonstrated. The same applies to the assay of simple drug formulations by any kind of methods and the determination of drugs in biological samples based merely on spiked samples. Drug purity/stability studies should contain information on the structure elucidation of the impurities/degradants.