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Validação do método de análise de enxofre por cromatografia
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O enxofre é um dos elementos químicos essenciais na agricultura, amplamente utilizado em produtos agroquímicos, especialmente fungicidas, para o controlo de doenças fúngicas que afetam culturas agrícolas. Além de ser antifúngico, o enxofre também possui outras propriedades tornando-o essencial para proteger plantações de diversas infeções, como o oídio. A quantificação rigorosa do enxofre é essencial para assegurar a eficácia do produto, em conformidade com os padrões industriais e regulamentares, garantindo simultaneamente a sua utilização segura. O presente trabalho desenvolvido na ASCENZA Agro S.A teve como objetivo validar o método de análise de enxofre por cromatografia de forma a permitir uma análise precisa do teor de enxofre. Propõe substituir métodos tradicionais como a titulação de iodo, no controlo de qualidade do produto. O método foi validado segundo os parâmetros exigidos pela norma ISO 17025, em vigor no laboratório em questão. Os resultados da validação concluíram que o método é bastante capaz de quantificar o teor de enxofre cumprindo-se os distintos critérios de aceitação estabelecidos. Para uma gama de trabalho de 0,004 mg/mL a 0,0016 mg/mL o método demonstrou-se linear com um coeficiente de correlação superior a 0,995, resíduos máximos inferiores a 10% e com ausência de outliers para todas as retas de calibração. Tendo em conta o padrão mais baixo, os valores de LD obtidos entre 0,0001 mg/mL e 0,0011 mg/mL e de LQ entre 0,0004 mg/mL e 0,0033 mg/mL são estatisticamente compatíveis com os valores experimentais. Quanto à precisão, o estudo das réplicas de amostras revelou uma média de amplitude relativa de 1,46% com uma variação de 1,29%, resultados aceites para este nível de concentração. A nível da justeza, as amostras reforçadas apresentaram taxas de recuperação média de 99,6%. Assim, esta validação representa um avanço significativo para o controle de qualidade no setor agroquímico, alinhando-se às necessidades de otimização dos processos industriais.
Sulfur is one of the essential chemical elements in agriculture, widely used in agrochemical products, especially fungicides, for controlling fungal diseases that affect crops. In addition to its antifungal properties, sulfur also possesses other characteristics that make it crucial for protecting plantations against various infections, such as oidium. Accurate quantification of sulfur is essential to ensure that the product meets the desired efficacy, complies with industrial and regulatory standards, and is used safely and effectively. This study, conducted at ASCENZA Agro S.A., aims to validate the sulfur analysis method using chromatography to enable precise sulfur content determination. It proposes replacing traditional methods such as iodine titration, as chromatography offers greater speed and efficiency in product quality control. The method was validated according to the parameters required by ISO 17025, the standard currently in force in the laboratory in question. The validation results confirmed that the method is highly capable of quantifying sulfur content with high accuracy and reliability, meeting the established acceptance criteria. For a working range of 0.004 mg/mL to 0.0016 mg/mL, the method demonstrated linearity with a correlation coefficient above 0.995, maximum residuals below 10%, and no outliers in any calibration curves. Considering the lowest standard, the obtained LD values between 0.0001 mg/mL and 0.0011 mg/mL and LQ values between 0.0004 mg/mL and 0.0033 mg/mL were statistically consistent with the experimental values. Regarding precision, the study of sample replicates revealed an average relative amplitude of 1.46%, with a variation of 1.29%, which is expected at this concentration level and methodology. Regarding accuracy, the spiked samples showed an average recovery rate of 99.6%. Thus, this validation represents a significant advancement in quality control within the agrochemical sector, aligning with the need for process optimization in industrial settings.
Sulfur is one of the essential chemical elements in agriculture, widely used in agrochemical products, especially fungicides, for controlling fungal diseases that affect crops. In addition to its antifungal properties, sulfur also possesses other characteristics that make it crucial for protecting plantations against various infections, such as oidium. Accurate quantification of sulfur is essential to ensure that the product meets the desired efficacy, complies with industrial and regulatory standards, and is used safely and effectively. This study, conducted at ASCENZA Agro S.A., aims to validate the sulfur analysis method using chromatography to enable precise sulfur content determination. It proposes replacing traditional methods such as iodine titration, as chromatography offers greater speed and efficiency in product quality control. The method was validated according to the parameters required by ISO 17025, the standard currently in force in the laboratory in question. The validation results confirmed that the method is highly capable of quantifying sulfur content with high accuracy and reliability, meeting the established acceptance criteria. For a working range of 0.004 mg/mL to 0.0016 mg/mL, the method demonstrated linearity with a correlation coefficient above 0.995, maximum residuals below 10%, and no outliers in any calibration curves. Considering the lowest standard, the obtained LD values between 0.0001 mg/mL and 0.0011 mg/mL and LQ values between 0.0004 mg/mL and 0.0033 mg/mL were statistically consistent with the experimental values. Regarding precision, the study of sample replicates revealed an average relative amplitude of 1.46%, with a variation of 1.29%, which is expected at this concentration level and methodology. Regarding accuracy, the spiked samples showed an average recovery rate of 99.6%. Thus, this validation represents a significant advancement in quality control within the agrochemical sector, aligning with the need for process optimization in industrial settings.
Descrição
Palavras-chave
Cromatografia líquida de alta eficiência Enxofre Validação Stulln WG Controlo de qualidade Validação de métodos analíticos