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Previous issue date: 2016-02-04 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / A ind?stria farmac?utica e laborat?rios anal?ticos de todo o mundo tem focado na qualidade, seguran?a e efic?cia de seus produtos. Processos utilizados para minimizar os riscos, como o Quality by Design (QbD), recentemente tem sido atribu?do ao desenvolvimento de m?todos anal?ticos, principalmente os m?todos cromatogr?ficos. O Analytical Quality by Design ou Qualidade Anal?tica Baseada no Projeto (aQbD), utiliza ferramentas de planejamento de experimentos, an?lise de risco e monitoramento cont?nuo. Para isso, faz-se uso de softwares simuladores, ferramentas estat?sticas e quimiom?tricas. Sabe-se que os m?todos cromatogr?ficos de an?lise s?o bastante consolidados e exigidos pelas ag?ncias regulat?rias, aplicando-se em diversas determina??es dentro do campo farmac?utico, como identifica??o e quantifica??o de f?rmacos, metab?litos, impurezas e produtos de degrada??o. O presente estudo teve como objetivo, utilizar ferramentas aQbD para o desenvolvimento de m?todos em cromatografia l?quida de ultra efici?ncia. Foram desenvolvidos quatro m?todos, a saber: quantifica??o simult?nea de dexametasona acetato e clotrimazol em formas farmac?uticas semiss?lidas, atrav?s de transfer?ncia de m?todo de CLAE para CLUE (cap?tulo 1); determina??o simult?nea de corticosteroides e conservantes em coluna de n?cleo s?lido com tamanho de part?cula 1.3 ?m utilizando software simulador (cap?tulo 2); quantifica??o de betametasona valerato em amostras de creme, gel, lo??o e pomada ap?s desenvolvimento de m?todo por planejamento fatorial completo 33 (cap?tulo 3); e determina??o simult?nea de corticosteroides ap?s desenvolvimento de modelo de previs?o de fator de reten??o por QSRR (cap?tulo 4). Os resultados mostraram que apesar da necessidade de otimiza??o pelo analista, o uso de ferramentas aQbD, como o planejamento estat?stico ou uso de softwares, s?o promissoras no desenvolvimento de m?todos cromatogr?ficos de ultra efici?ncia, uma vez que foram capazes de promover economia de tempo, diminuir os gastos e riscos. Os ensaios apresentaram resultados satisfat?rios em termos de velocidade anal?tica e diminui??o no consumo de solventes. / The pharmaceutical industry and analytical laboratories around the world have focused
on quality, safety and efficacy of their products. Processes used to minimize risks, such as
Quality by Design (QbD), which recently has been attributed to the development of analytical
methods, especially chromatographic methods. The Analytical Quality by Design (aQbD)
uses planning tools experiments, risk analysis and continuous monitoring. For this, it makes
use of simulation software, statistical tools and chemometrics.
It is known that chromatographic methods are well consolidated and required by the
regulatory agencies. It has been applied in various determinations in the pharmaceutical field,
such as identification and quantification of drugs, metabolites, degradation products and
impurities. The aim of this study was to use aQbD tools for the development of methods for
ultra high performance liquid chromatography (UHPLC). Four methods were developed,
namely: simultaneous quantification of dexamethasone acetate and clotrimazole in semisolid
dosage forms, via HPLC to UHPLC method transfer (Chapter 1); simultaneous determination
of corticosteroids and preservatives in solid core column with particle size of 1.3 ?m by using
simulation software (Chapter 2); betamethasone valerate quantification in samples of cream,
gel, lotion and ointment after method development by full factorial design 33 (Chapter 3); and
simultaneous determination of corticosteroids after retention factor prediction model by
QSRR (Chapter 4).
The results showed that despite the need for optimization by the analyst, the use of
aQbD tools such as statistical design or use of software, the aQbD is promising in the
development of chromatographic methods of ultra efficiency, since they were able to promote
time savings, lower costs and risks. The tests showed satisfactory results in terms of analysis
speed and decrease of solvent consumption.
| Identifer | oai:union.ndltd.org:IBICT/oai:repositorio.ufrn.br:123456789/21438 |
| Date | 04 February 2016 |
| Creators | Solon, Lilian Grace da Silva |
| Contributors | 62001728468, http://lattes.cnpq.br/9657118649043311, Barbosa, Euz?bio Guimar?es, 94373531153, http://lattes.cnpq.br/3197108792266393, Nogueira, Fernando Henrique Andrade, 03830430698, http://lattes.cnpq.br/3818421971151621, Souza, F?bio Santos de, 92771300400, http://lattes.cnpq.br/4903883301058477, Navarro, Marco Vinicius Monteiro, 32851146491, http://lattes.cnpq.br/4867451742538033, Scotti, Marcus Tullius, 25514316890, http://lattes.cnpq.br/9312500923026323, Arag?o, Cicero Fl?vio Soares |
| Publisher | PROGRAMA DE P?S-GRADUA??O EM DESENVOLVIMENTO E INOVA??O TECNOL?GICA EM MEDICAMENTOS, UFRN, Brasil |
| Source Sets | IBICT Brazilian ETDs |
| Language | Portuguese |
| Detected Language | English |
| Type | info:eu-repo/semantics/publishedVersion, info:eu-repo/semantics/doctoralThesis |
| Source | reponame:Repositório Institucional da UFRN, instname:Universidade Federal do Rio Grande do Norte, instacron:UFRN |
| Rights | info:eu-repo/semantics/openAccess |
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