Determinação de impurezas inorgânicas em medicamentos: avaliação de preparo de amostra e medidas espectroanalíticas

• Ano de defesa: 2021
• Autor(a) principal: Pinheiro, Fernanda Costa
• Orientador(a): Nóbrega, Joaquim de Araújo
• Tipo de documento: Tese
• Tipo de acesso: Acesso aberto
• Idioma: eng
• Instituição de defesa: Universidade Federal de São Carlos; Câmpus São Carlos
• Programa de Pós-Graduação: Programa de Pós-Graduação em Química - PPGQ
• Palavras-chave em Inglês: Microwave-assisted digestion; Dispersive liquid-liquid microextraction; Calibration methods; Spectroanalytical techniques; United States Pharmacopoeia
• Área do conhecimento CNPq: CIENCIAS EXATAS E DA TERRA::QUIMICA
• Link de acesso: https://repositorio.ufscar.br/handle/20.500.14289/14567

Green sample preparation procedures were developed in this dissertation for determination of elemental impurities in drugs and dietary supplements by argon-based plasma spectroanalytical methods according to Chapters 232, 233 and 2232 from the United States Pharmacopeia. Chapter 3 describes the development of a procedure for microwave-assisted sample preparation of medicines using diluted nitric acid solution followed by determination of 24 elements using inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS). A dispersive liquid-liquid microextraction procedure for determination of Cd, Hg, and Pb in drug samples by ICP OES is also presented. A dilute-and-shoot procedure for determination of 23 elements in liquid pharmaceutical samples by ICP OES is presented in Chapter 4 as well as a procedure for dispersive liquid-liquid microextraction of Cd, Co, Hg, Ni, Pb, and V in liquid drug samples for subsequent measurements by ICP OES. Chapter 5 describes the development of microwave-assisted sample preparation procedure of sport supplements using dilute nitric acid solution followed by determination of As, Cd, Hg and Pb using ICP-MS. In all chapters previously mentioned, calibration strategies, such as standard additions, internal standardization, multi-isotope calibration and one-point standard addition, are evaluated for correction of matrix effects as well as instrumental strategies based on aerosol dilution and collision cell technology for ICP-MS measurements. These strategies were essential to correct for spectral and non-spectral interferences, enabling the accurate determination of elemental impurities in solid pharmaceutical samples (tablets and pills), liquid drugs (oral solutions and parenteral drugs) and sport supplements by ICP-based methods.