validação de métodos para determinação dos ácidos fítico e oxálico em multimistura validation methods to determine phytic and oxalic acids in "multimisturas"
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ID: 221136
2006
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Abstract
Considerando a composição da multimistura distribuída em Belo Horizonte/MG (trigo, fubá, casca de ovo e folha de mandioca), as metodologias de detecção e/ou quantificação dos fitatos e oxalatos foram validadas. A purificação em coluna de troca aniônica forte do ácido fítico e seus derivados desfosforilados extraídos da multimistura apresentou baixos valores de recuperação (49%) nas concentrações menores do fitato adicionado, em relação às mais elevadas (101%), sugerindo a interferência de minerais presentes em altas concentrações, principalmente cálcio. Dos métodos avaliados para a determinação do ácido oxálico, a cromatografia de exclusão iônica foi a que apresentou os melhores resultados, com boas recuperações nos níveis mais altos de adição (88%), apresentando, contudo, recuperação mais baixa nos níveis inferiores de adição (61%). Os teores de ácido fítico nas amostras variaram de 1,61 g/100 g a 2,25 g/100 g e, para o ácido oxálico, de 0,044 g/100 g a 0,057 g/100 g. Os critérios de validação dos métodos analíticos por cromatografia líquida de alta eficiência foram considerados satisfatórios quanto a seletividade e especificidade, linearidade, repetitividade e limites de detecção e quantificação. Contudo, o de recuperação não foi atendido satisfatoriamente, visto que as porcentagens obtidas foram inferiores ao esperado, levando-se em conta a concentração adicionada nas amostras.
Taking into account the composition of the "multimistura" distributed in Belo Horizonte/MG (wheat, corn meal, egg shell and cassava leave), the methods of detection and/or quantitation of phytates and oxalates were validated. The purification of phytic acid and its dephosphorylated derivatives extracted from the "multimistura" using a strong anionic exchange column presented low values of recovery (49%) at low concentrations of the added phytate, when related to the higher ones (101%), which suggests interference of minerals present in high levels, mainly calcium. From the methods evaluated for the determination of oxalic acid, the ionic exclusion chromatography was the one that presented the best results, with good recoveries at the highest addition levels (88%); presenting, however, decreased recovery in the lower levels of addition (61%). The levels of phytic acid in the samples varied from 1.61 g/100 g to 2.25 g/100 g and for the oxalic acid, from 0.044 g/100 g to 0.057 g/100 g. The validation criteria for the analytical methods by high performance liquid chromatography were considered satisfactory for selectivity and specificity, linearity, repetitivity and limits of detection and quantitation. However, the recovery was not satisfactory since the obtained percentages were lower than the expected one, taking into account the quantities added to the samples.
Taking into account the composition of the "multimistura" distributed in Belo Horizonte/MG (wheat, corn meal, egg shell and cassava leave), the methods of detection and/or quantitation of phytates and oxalates were validated. The purification of phytic acid and its dephosphorylated derivatives extracted from the "multimistura" using a strong anionic exchange column presented low values of recovery (49%) at low concentrations of the added phytate, when related to the higher ones (101%), which suggests interference of minerals present in high levels, mainly calcium. From the methods evaluated for the determination of oxalic acid, the ionic exclusion chromatography was the one that presented the best results, with good recoveries at the highest addition levels (88%); presenting, however, decreased recovery in the lower levels of addition (61%). The levels of phytic acid in the samples varied from 1.61 g/100 g to 2.25 g/100 g and for the oxalic acid, from 0.044 g/100 g to 0.057 g/100 g. The validation criteria for the analytical methods by high performance liquid chromatography were considered satisfactory for selectivity and specificity, linearity, repetitivity and limits of detection and quantitation. However, the recovery was not satisfactory since the obtained percentages were lower than the expected one, taking into account the quantities added to the samples.
| Reference Key |
nappi2006foodvalidao
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| Authors | ;Giancarlo Ubaldo Nappi;Mariem Rodrigues Ribeiro-Cunha;José Virgílio Coelho;Lieselotte Jokl |
| Journal | software - practice and experience |
| Year | 2006 |
| DOI |
10.1590/S0101-20612006000400016
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