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Comprehensive analysis of vitamin D3 impurities in oily drug products using supercritical fluid chromatography-mass spectrometry.
Jambo, Hugues; Dispas, Amandine; Pérez-Mayán, Leticia; Rodríguez, Isaac; Ziemons, Éric; Hubert, Philippe.
Afiliación
  • Jambo H; Laboratory of Pharmaceutical Analytical Chemistry, CIRM, ScF-Santé hub, University of Liège (ULiège), Liège, Belgium.
  • Dispas A; Laboratory of Pharmaceutical Analytical Chemistry, CIRM, ScF-Santé hub, University of Liège (ULiège), Liège, Belgium.
  • Pérez-Mayán L; Laboratory for the Analysis of Medicines, CIRM, University of Liège (ULiège), Liège, Belgium.
  • Rodríguez I; Department of Analytical Chemistry, Nutrition and Food Sciences, Research Institute on Chemical and Biological Analysis (IAQBUS), Universidade de Santiago de Compostela, Santiago de Compostela, Spain.
  • Ziemons É; Department of Analytical Chemistry, Nutrition and Food Sciences, Research Institute on Chemical and Biological Analysis (IAQBUS), Universidade de Santiago de Compostela, Santiago de Compostela, Spain.
  • Hubert P; Laboratory of Pharmaceutical Analytical Chemistry, CIRM, ScF-Santé hub, University of Liège (ULiège), Liège, Belgium.
Drug Test Anal ; 16(7): 692-707, 2024 Jul.
Article en En | MEDLINE | ID: mdl-38482734
ABSTRACT
Vitamin D3, an essential micronutrient, often requires supplementation via medicines or food supplements, which necessitate quality control (QC). This study presents the development of a method for detecting and quantifying seven impurities of vitamin D3 in oily drug products using supercritical fluid chromatography-mass spectrometry (SFC-MS). Targeted impurities include two esters of vitamin D3 and five non-esters including four that are isobaric to vitamin D3. Firstly, a screening study highlighted the Torus 1-AA column and acetonitrile modifier as adequate for the separation, followed by optimization of the SFC conditions. Secondly, make-up solvent composition and MS settings were optimized to reach high sensitivity. For both the separation and MS response, the screening design of experiments proved useful. Lastly, a fast saponification and liquid-liquid extraction method was developed, enabling efficient sample cleanup and impurities recovery from the complex oily matrix. The SFC-MS method suitability was assessed in two validation studies. The first study employed the ICH Q2 guideline for impurity limit test to demonstrate method specificity and establish a limit of detection (LOD) and a limit of quantification (LOQ) at 0.2% and 0.5%, respectively, for ester impurities. The second study conducted a comprehensive quantitative assessment for three non-ester impurities using a total error approach, determining method validity through accuracy profiles. The validated method exhibited reliable performance across impurity concentrations from 0.1% to 2.0%, with estimated LODs ranging from 2 to 7 ng/mL. This study further promotes SFC-MS as a valuable, versatile, and green tool for routine pharmaceutical QC.
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Texto completo: 1 Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Contaminación de Medicamentos / Colecalciferol / Cromatografía con Fluido Supercrítico / Límite de Detección Idioma: En Revista: Drug Test Anal Asunto de la revista: FARMACOLOGIA Año: 2024 Tipo del documento: Article País de afiliación: Bélgica Pais de publicación: Reino Unido
Texto completo
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Texto completo: 1 Colección: 01-internacional Base de datos: MEDLINE Asunto principal: Contaminación de Medicamentos / Colecalciferol / Cromatografía con Fluido Supercrítico / Límite de Detección Idioma: En Revista: Drug Test Anal Asunto de la revista: FARMACOLOGIA Año: 2024 Tipo del documento: Article País de afiliación: Bélgica Pais de publicación: Reino Unido