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Master's Dissertation
DOI
https://doi.org/10.11606/D.85.2016.tde-22082016-150806
Document
Author
Full name
Cláudio Leão
E-mail
Institute/School/College
Knowledge Area
Date of Defense
Published
São Paulo, 2016
Supervisor
Committee
Bustillos, José Oscar Willian Vega (President)
Parra, Duclerc Fernandes
Rossini, Edvaldo Luis
Title in Portuguese
Desenvolvimento e validação de metodologia para a determinação de monocloroacetato de sódio e dicloroacetato de sódio em cocoamido,N-[(3-dimetilamino)propil],betaína via cromatografia a gás: GC/FID, GC/ECD e GC/MS
Keywords in Portuguese
anfótero
cloroacetato
cromatografia
surfactante
Abstract in Portuguese
O monocloroacetato de sódio (MCAS) e o dicloroacetato de sódio (DCAS) são compostos tóxicos e irritantes ao ser humano e nocivos ao meio ambiente, sendo impurezas indesejáveis na cocoamido propil betaína (CAPB), que é um surfactante anfótero utilizado em produtos de consumo dos segmentos cosmético e domiciliar. Diante dos requisitos de concentração em nível de mg/kg exigidos pelos órgãos reguladores de saúde do governo, tornou-se mandatório o emprego de metodologia com limite de quantificação, precisão e exatidão adequados aos rígidos controles de processo pelos fabricantes da CAPB, bem como, dispor de técnicas convencionais com poder de resolução e proficiência pelo controle de qualidade e neste contexto inseriu-se a cromatografia a gás. Neste estudo foram estabelecidos os procedimentos analíticos que definiram as melhores condições para identificar e quantificar as impurezas MCAS e DCAS na matriz CAPB por meio da cromatografia a gás. A preparação das amostras consistiu da derivação das impurezas MCAS e DCAS a ésteres etílicos e a extração líquido-líquido em hexano para separar dos demais constituintes da matriz. Os modos de detecção acoplados à cromatografia a gás foram a ionização pela chama (GC/FID), a captura de elétrons (GC/ECD) e a espectrometria de massas (GC/MS). A validação comprovou que as metodologias são lineares entre 4 e 50 mg/kg com recuperação de 70 a 120%, apresentam limites de quantificação inferiores a 10 mg/kg e produziram médias e incertezas similares na amostra examinada, constituindo-se alternativas para a determinação de cloroacetatos em betaínas.
Title in English
Development and validation of method for determination of sodium monochloroacetate and sodium dichloroacetate in cocoamide,N-[(3-dimethylamine)propyl],betaine by gas chromatography: GC/FID, GC/ECD e GC/MS
Keywords in English
amphoteric
chloroacetate
chromatography
surfactant
Abstract in English
The sodium monochloroacetate (MCAS) and the sodium dichloroacetate (DCAS) are toxic and irritating compounds to humans and harmful to the environment, being undesirable impurities in cocoamidepropyl betaine (CAPB), which is a amphoteric surfactant used in consumer products of cosmetic and household segments. Considering the content requirements at level mg/kg defined by governmental health agency, became mandatory the use of analytical methods with appropriate precision, accuracy and quantification limit to rigid process controls by CAPB manufacturers, as well as, to have available conventional techniques with good resolution and proficiency for quality control staff and in this context was inserted the gas chromatography. In this study, the analytical procedures were established to define the best conditions to identify and quantify the impurities MCAS and DCAS in CAPB matrix by gas chromatography. The sample preparation consisted of MCAS and DCAS derivation to ethyl esters and liquid-liquid extraction in hexane to separate them from the other constituents of matrix. The detection modes coupled to gas chromatography were the flame ionization (GC/FID), electron capture (GC/ECD) and mass spectrometry (GC/MS). The validation ensured that the methodologies are linear between 4 and 50 mg/kg with recovery 70 to 120%, presents quantification limits less than 10 mg/kg and produced similar averages and uncertainties in the examined sample, constituting an alternative for determination of chloroacetates in betaines.
 
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Publishing Date
2016-08-25
 
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