I. GENERALITES
1.6. Méthodes contraceptives
O método proposto foi aplicado na determinação de arsênio, em amostras de vinho adquiridas em supermercados de Salvador. Foram analisadas 20 amostras vinho de diferentes regiões do Brasil. Os resultados encontram-se expostos na Tabela 5.6, com suas respectivas concentrações e intervalos de confiança para cada uma das amostras.
A Figura 5.3 mostra uma distribuição uniforme dos resultados de arsênio total em vinhos brasileiros. Estes resultados demonstram que as concentrações de arsênio, encontradas nas amostras, estão dentro do limite estabelecido pelo Decreto Federal n° 99.066/90 da lei 7.678/88 do Ministério da Agricultura.
Tabela 5.6 Determinação de arsênio total em amostras de vinhos comercializadas no
Brasil.
Tipo Origem Tipo de Uva As (µg L-1)
Tinto seco São Francisco Cabernet Sauvignon 14,1 ± 1,2
Tinto seco São Francisco Shiraz 12,7 ± 0,8
Branco seco Bento Gonçalves Chardonnay 15,5 ± 1,7
Branco seco São Francisco Chenin Blanc 10,1 ± 0,6
Tinto demi-seco São Francisco Tannat 19,1 ± 0,5
Branco demi-seco Campanha Riesling 13,6 ± 1,0
Tinto suave Caxias do Sul 10,3 ± 1,0
Branco suave Bento Gonçalves 9,9 ± 0,7
Tinto seco Santana do Livramento Cabernet Franc 14,3 ± 0,9
Branco Seco Bento Gonçalves Chardonnay 17,2 ± 1,4
Tinto demi seco S. Bernado do Campos Cabernet Franc 16,1 ± 1,2 Tinto seco fino Santana do Livramento Merlot 10,4 ± 0,7
Branco seco São Francisco Chenin Blanc 18,4 ± 0,9
Tinto seco Caxias do Sul Cabernet Sauvignon 12,8 ± 0,6 Tinto seco Bento Gonçalves Cabernet Sauvignon,
Merlot e Pinot Noir
9,9 ± 0,8
Tinto seco Caxias do Sul Tannat 13,5 ± 1,0
Tinto seco Bento Gonçalves Gamay 8,7 ± 0,8
Tinto suave São Francisco Cabernet Sauvignon e Shiraz
15,3 ± 0,7 Branco suave São Francisco Moscato Canelli 16,9 ± 0,6
5.4. Considerações Finais
A otimização multivariada, utilizando-se planejamento Box - Behnken, permitiu uma rápida e eficiente otimização das condições de geração de hidretos.
Os valores obtidos dos parâmetros de mérito (Tabela 5.4) comprovam que o método tem sensibilidade suficiente para ser aplicado na avaliação do teor de arsênio, em vinhos brasileiros, com as vantagens de ser simples, de baixo custo e fácil manipulação, podendo ser aplicado na determinação rotineira do metal com LQ de 0,2 g L-1.
As amostras analisadas apresentaram concentração de arsênio na faixa de 8,7 a 19,1 g L-1. Estes resultados estão de acordo com os encontrados na literatura [269] e estão abaixo do limite máximo permitido pela Organização Internacional da Vinha e do Vinho (OIV), pelo Ministério da Agricultura do Brasil (Decreto Federal n° 99066/90) e pelo Mercosul, 0,2 mg L-1.
Considerações Finais da Tese
A introdução das amostras, através do sistema termospray, melhorou significativamente a sensibilidade do FAAS.
O desempenho do TS-FF-AAS foi melhorado ainda mais com o uso do sistema de pré-concentração, em fase sólida com uma minicoluna de XAD- 7, carregada com ditizona. Os limites de detecção obtidos, 0,012 e 0,34 µg L-1 para cádmio e chumbo respectivamente, são comparáveis com os encontrados pelo ET AAS, sendo que a técnica TS-FF-AAS apresenta custo de operação menor que a do ET AAS.
O procedimento de pré-concentração de íons cádmio e chumbo, por meio da extração em fase sólida, permitiu uma separação eficiente da matriz estudada. A otimização multivariada, utilizando-se o planejamento Box - Behnken, proporcionou uma rápida e eficiente otimização do procedimento de pré-concentração proposto.
A análise de especiação não-cromatográfica é uma alternativa simples e de baixo custo, quando comparada com a análise cromatográfica, para determinação de espécies de arsênio e antimônio, em amostras de alimentos.
Os procedimentos de extração de espécies de arsênio e antimônio, em amostras de vegetais, empregando ácido sulfúrico mostraram-se bastante eficientes para as amostras analisadas.
As técnicas analíticas empregadas, com geração de hidretos, são muito sensíveis para determinação de quantidades traço de arsênio e antimônio. A separação do analito da amostra elimina o efeito de matriz, aumentando a sensibilidade e diminuindo o limite de detecção. Os limites de quantificação obtidos para as espécies de arsênio e antimônio: 2,0, 3,6, 2,8 e 4,7 ng g -1 para Sb (III), Sb (V), As (III) e As (V), respectivamente, juntamente com a boa exatidão e precisão do método, comprovam que o mesmo pode ser aplicado na determinação destes metalóides, nas amostras analisada, através da espectrometria de fluorescência atômica com geração de hidreto.
A HG AAS com atomização eletrotérmica mostrou-se uma técnica sensível para determinação de arsênio total em amostras de vinhos: O LQ de 0,2 µg L-1, o baixo custo e a fácil manipulação que o método permite, demonstra a aplicabilidade do mesmo, para avaliação do teor de arsênio em vinhos brasileiros.
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