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Caracterizações físico-químicas de formulações híbridas
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No presente projeto, caracterizam-se físico-quimicamente quatro protótipos de soluções
concentradas (RD_A, RD_B, RD_C, RD_D) com o objetivo de verificar qual apresentava os resultados
mais promissores de acordo com as especificações exigidas pelas entidades reguladoras, nomeadamente
Organização das Nações Unidas para a Alimentação e a Agricultura, SANCO e a Comissão Europeia, e
definidas pela Ascenza. Foram ainda aplicadas técnicas analíticas para a caracterização do produto
técnico utilizado para formular os quatro protótipos.
Numa primeira abordagem, para as caracterizações físico-químicas recorreu-se a métodos
estabelecidos pelo Conselho Analítico Colaborativo de Pesticidas Internacionais, mas também a
métodos desenvolvidos no laboratório de Deformulação, nomeadamente para obter o teor de substância
ativa no formulado. No que se refere aos quatro protótipos, estes foram caracterizados quer à
temperatura ambiente, quer após 14 dias em estufa (54 ºC), com o objetivo de simular o período de
validade de dois anos, aplicando-se diferentes técnicas, designadamente a determinação do pH,
persistência de espumas, tensão superficial, densidade, estabilidades de emulsão e solução diluída. À
exceção dos protótipos RD_A, no qual os valores da espuma e pH foram superiores aos previstos, e
RD_D em que a espuma foi superior ao estipulado pela Ascenza, os restantes valores dos quatro
formulados estão de acordo com o previamente estabelecido.
O teor de substância ativa presente em cada formulado, foi determinado por cromatografia
líquida de ultra eficiência com detetor por rede de díodos, tendo sido possível verificar que para além
do protótipo RD_C, todos os outros apresentaram as especificações exigidas tanto pelas entidades
reguladoras, tanto pela Ascenza. Com base nesta técnica determinou-se o teor da substância ativa
presente no produto técnico utilizado para produzir os protótipos, tendo sido de aproximadamente 95%,
valor dentro do expectável.
Em relação ao produto técnico, foi possível verificar através das diferentes técnicas,
nomeadamente Espetroscopia de infravermelho com transformada de Fourier, Termogravimetria
combinada com a calorimetria diferencial de varrimento e Cromatografia líquida acoplada a
espetrometria de massa tandem, que este era constituído maioritariamente pela substância ativa em
estudo. Através da Espetroscopia de infravermelho com transformada de Fourier constatou-se que havia
uma correspondência de 0,9883 com o padrão analítico, e que as bandas existentes eram características
da substância ativa. Na Termogravimetria combinada com a calorimetria diferencial de varrimento foi
possível verificar que o ponto de fusão do produto técnico (98,6 ºC) se encontra próximo do valor
referência (98,9ºC). Quanto à Cromatografia líquida acoplada a espetrometria de massa tandem, à
energia de 15 eV, foi possível observar algumas das fragmentações características da molécula em
estudo, reforçando, assim, que o produto técnico é composto maioritariamente por esta substância ativa.
Em suma, com base nas técnicas desenvolvidas e aplicadas, foi assim possível concluir que o
protótipo RD_B é o que evidencia resultados mais concordantes com as especificações estabelecidas
pelas entidades reguladoras e pela Ascenza. No que diz respeito ao produto técnico, conclui-se ser
constituído maioritariamente pela molécula em estudo.
In this work were characterized the physico-chemical properties of four prototypes of soluble concentrates, (RD_A, RD_B, RD_C, RD_D) with the objective to check which one had the most promising results based in the specifications required by the regulatory authorities, namely Food and Agriculture Organization of the United Nations, SANCO, and European Commission, and defined by Ascenza. Various analytical techniques were used to characterize technical product present in the soluble concentrate and to characterize the final formulated prototypes. In a first approach, for physico-chemical characterizations were used methods established by Collaborative International Pesticides Analytical Council and, also methods developed internally by the Deformulation Laboratory. The four prototypes were characterized at room temperature, and after 14 days under 54 ºC (with the goal to simulate the validity period), applying different techniques, in particular determination of pH, persistence of foam, surface tension, density, emulsion stability and dilution stability. Except for prototype RD_A, which the values of pH and persistence of foam were higher than expected, and RD_D which persistence of foam was out of the specification established by Ascenza, the other values of four prototypes were in accordance with what was established. Regarding the content of active ingredient present in each formulated soluble concentrate, it was determined by liquid chromatography. From the results obtained, it was concluded that, except for RD_C, where the values were above specification, the other prototypes comply with the specification established by authorities and Ascenza. It was also determined the content of active ingredient present in technical product, and value obtained was 95%. Concerning the technical product, different techniques such as Fourier-transform infrared spectroscopy, Thermogravimetry and Differential Scanning Calorimetry, and Liquid Chromatography with tandem mass spectrometry, were used for its characterization. Via Fourier-transform infrared spectroscopy, it was possible to verify the bands characteristic of the molecule, and a match of 0.9883 was obtain when comparing the technical product to an analytical standard. In Thermogravimetry and Differential Scanning Calorimetry, it was possible to observe that melting point of technical product (98,6 ºC) was close to the reference value (98,9 ºC). In Liquid Chromatography with tandem mass spectrometry, at an energy of 15 eV, it was observed some characteristic fragmentations of the molecule, emphasizing that the technical product is mainly composed by the active ingredient. To conclude, according to the above techniques, it was possible conclude that RD_B prototype is the one which shows the most compliant results with the specifications defined by the authorities and Ascenza. In relation to technical product, we may conclude that it is mainly composed by ative ingredient.
In this work were characterized the physico-chemical properties of four prototypes of soluble concentrates, (RD_A, RD_B, RD_C, RD_D) with the objective to check which one had the most promising results based in the specifications required by the regulatory authorities, namely Food and Agriculture Organization of the United Nations, SANCO, and European Commission, and defined by Ascenza. Various analytical techniques were used to characterize technical product present in the soluble concentrate and to characterize the final formulated prototypes. In a first approach, for physico-chemical characterizations were used methods established by Collaborative International Pesticides Analytical Council and, also methods developed internally by the Deformulation Laboratory. The four prototypes were characterized at room temperature, and after 14 days under 54 ºC (with the goal to simulate the validity period), applying different techniques, in particular determination of pH, persistence of foam, surface tension, density, emulsion stability and dilution stability. Except for prototype RD_A, which the values of pH and persistence of foam were higher than expected, and RD_D which persistence of foam was out of the specification established by Ascenza, the other values of four prototypes were in accordance with what was established. Regarding the content of active ingredient present in each formulated soluble concentrate, it was determined by liquid chromatography. From the results obtained, it was concluded that, except for RD_C, where the values were above specification, the other prototypes comply with the specification established by authorities and Ascenza. It was also determined the content of active ingredient present in technical product, and value obtained was 95%. Concerning the technical product, different techniques such as Fourier-transform infrared spectroscopy, Thermogravimetry and Differential Scanning Calorimetry, and Liquid Chromatography with tandem mass spectrometry, were used for its characterization. Via Fourier-transform infrared spectroscopy, it was possible to verify the bands characteristic of the molecule, and a match of 0.9883 was obtain when comparing the technical product to an analytical standard. In Thermogravimetry and Differential Scanning Calorimetry, it was possible to observe that melting point of technical product (98,6 ºC) was close to the reference value (98,9 ºC). In Liquid Chromatography with tandem mass spectrometry, at an energy of 15 eV, it was observed some characteristic fragmentations of the molecule, emphasizing that the technical product is mainly composed by the active ingredient. To conclude, according to the above techniques, it was possible conclude that RD_B prototype is the one which shows the most compliant results with the specifications defined by the authorities and Ascenza. In relation to technical product, we may conclude that it is mainly composed by ative ingredient.
Descrição
Tese de mestrado, Química (Química), 2022, Universidade de Lisboa, Faculdade de Ciências
Palavras-chave
formulado substância ativa produto fitofarmacêutico caracterização analítica solução concentrada Teses de mestrado - 2022