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Master's Dissertation
DOI
10.11606/D.9.2017.tde-26092017-171859
Document
Author
Full name
Angel Arturo Gaona Galdos
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Paulo, 2008
Supervisor
Committee
Kedor, Erika Rosa Maria (President)
Lopez, Renata Fonseca Vianna
Tavares, Marina Franco Maggi
Title in Portuguese
Desenvolvimento de metodologia analítica específica e seletiva para a determinação do nitrato de econazol em cremes
Keywords in Portuguese
Controle físico-químico de qualidade dos fármacos
Creme (Controle de qualidade)
Formas farmacêuticas (Análise qualitativa; Análise quantitativa)
Abstract in Portuguese
Neste trabalho realizaram-se provas de identificação qualitativa e quantitativa do nitrato de econazol (matéria-prima); ensaios de caracterização térmica do nitrato de econazol, excipientes e formulação farmacêutica (creme), assim como desenvolvimento de metodologia analítica específica e seletiva para a quantificação do nitrato de econazol na formulação farmacêutica de creme. A caracterização térmica dos excipientes foi realizada usando-se a Termogravimetria (TG). Para a caracterização térmica do nitrato de econazol e da formulação foram empregadas a Termogravimetria, a Termogravimetria Derivada (TG/DTG) e a Calorimetria Exploratória Diferencial (DSC). Na caracterização térmica da formulação foram identificados e quantificados dois tipos de água com interações diferentes com a matriz. No desenvolvimento da metodologia específica utilizou-se a eletroforese capilar em zona, método linear com concentrações entre 80 e 120 µg mL-1, com coeficiente de correlação de 0,9995; precisão calculada como desvio padrão relativo (DPR) menor de 2%; exatidão do método comprovada mediante teste de recuperação, obtendo-se valores de 100±2,5%; limites de detecção e quantificação 1,853 µg.mL-1 e 5,617 µg.mL-1, respectivamente, comprovando-se também que o método é robusto. No desenvolvimento da metodologia seletiva foram usadas a cromatografia líquida de alta eficiência com eluição em gradiente (CLAE) e a eletroforese capilar pelo método da cromatografia eletrocinética micelar (MEKC). Nestes métodos foram separados o nitrato de econazol, as impurezas relatadas na literatura do nitrato de econazol (4-álcool clorobenzílico, alfa-2,4-diclorofenil-1 H¬imidazol-1-etanol) e os conservantes presentes na formulação (metilparabeno e propilparabeno). O método seletivo desenvolvido por CLAE foi linear para todas as moléculas, com coeficientes de correlação maiores de 0,99. A precisão calculada para o nitrato de econazol como DPR foi menor de 2%; a exatidão para o nitrato de econazol foi comprovada mediante teste de recuperação, obtendo-se valores de 100±2%; comprovou-se também que o método é robusto e que poderia ser aplicado para a quantificação de cada um destes cinco compostos. No método seletivo desenvolvido por MEKC se obteve tempo menor em comparação ao método por CLAE.
Title in English
Development of a specific and selective analytical methodology for the determination of econazole nitrate in creams
Keywords in English
Creme (Quality control)
Pharmaceutical forms (Qualitative analysis; Quantitative analysis)
Physical-chemical control of drug quality
Abstract in English
In this work, were performed qualitative and quantitative identitication econazole nitrate (raw material); thermal characterization of econazole nitrate, excipients and formulation (cream). There also were developed and validated specific and selective analytical methodology for quantitative determination of econazole nitrate in creams. The thermal characterization of drug product excipients was performed using the Thermogravimetry (TG). For the thermal characterization of econazole nitrate drug and their formulation were used the Thermogravimetry, Derivative Thermogravimetry (TG/DTG) and Differential Scanning Calorimetry (DSC). From cream formulation were identified and quantified two kinds of water which have different interactions with matrix. As regards lo developing of specific methodology was used the capillary zone electrophoresis (CZE). The method was linear, with a correlation coefficient of 0.9995 in the concentration range of 80 to 120 µg.mL-1 of econazole nitrate, precision calculated as relative standard deviation (RSD) was less than 2%, accuracy calculated percentage of recovery for commercial sample was of 100 ± 2.5%, detection and quantitation limits were 1.853 µg.mL-1 and 5.617 µg.mL-1, respectively. The CZE method showed to be robust. For developing of selective methodology were used high performance liquid chromatography (HPLC) with gradient elution, and micellar electrokinetic chromatography (MEKC) methods. Econazole nitrate, related impurities the drug (4-Chlorobenzyl alcohol, alpha-2,4-dichlorophenyl-1H - imidazole-1-ethanol) and preservatives (methylparaben, propylparaben) present in the drug product were separated. The HPLC method was linear for all analytes, the correlation coefficients were higher than 0.99. The precision for nitrate econazol in terms of RSD was less than 2%, the percentage of recovery for commercial sample of econazole nitrate was 100±2%, the method is robust and could be applied for the quantitation of the five substances cited above. With the MEKC method developed the five substances were separated less time comparated with HPLC method.
 
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Publishing Date
2017-09-26
 
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