Development of analyrtical methods for determination of N-nitrosamines in shampoo samples by liquid chromatography coupled to diode array, electrochemical and mass spectrometry detecto / Desenvolvimento de métodos para determinação de N-nitrosaminas em amostras de xampu por cromatografia líquida acoplada à detecção por arranjo de diodos, eletroquímica e espectrometria de massas

AUTOR(ES)
FONTE

IBICT - Instituto Brasileiro de Informação em Ciência e Tecnologia

DATA DE PUBLICAÇÃO

21/02/2011

RESUMO

N-nitrosamines (NA) are N-nitroso compounds, showed to be carcinogenic in a wide variety of experimental animals. In addition, they also present mutagenic and teratogenic activities. N-nitrosamines have been found during the last three decades in a variety of consumer products, including cosmetic and personal care products, and their raw materials. The most common NA detected in cosmetics were N-nitrosodiethanolamine (NDELA), N-nitrosomorpholine (NMOR) and Nnitrosodimethylamine (NDMA), in concentrations varying from mg kg to mg kg. The aims of this work were the evaluation of the electrochemical behavior of NA on a boron doped diamond electrode and construction of an amperometric cell to be coupled to high performance liquid chromatography (HPLC), as well as the development and validation of methods for determination of NA in shampoo, using liquid chromatography coupled to the developed electrochemical cell, photodiode array and mass spectrometry detectors. The electrochemical behavior of NA was studied using cyclic voltammetry and square wave voltammetry; composition, concentration and pH of the electrolyte were evaluated. The separation of NA was achieved using a C18 XBridge¿ column and mobile phase of water and acetonitri le under gradient elution. For sample preparation liquid-liquid extraction, solid phase extraction (C18 and silica) and matrix solid phase dispersion were evaluated. The performance of the different detectors coupled to liquid chromatography to the NA determination in shampoo was compared. Finally, a liquid-chromatography-mass spectrometry method was validated to the determination of NMOR and NDMA in shampoo, thorough the following parameters: linear range, linearity, intra-day and inter-day precision, selectivity, limit of detection, limit of quantification and accuracy. The method was applied to the determination of NA in shampoo samples

ASSUNTO(S)

mass spectrometry n-nitrosaminas xampu cromatografia líquida espectrometria de massa n-nitrosamines shampoo liquid chromatography

ACESSO AO ARTIGO

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