Abstract This chapter describes fundamentals and applications of design of experiments (DOE) empl... more Abstract This chapter describes fundamentals and applications of design of experiments (DOE) employed for the method development of sample preparation using solid phase extraction. During method optimization, the presence of a large number of variables (factors) can become a critical step. Thus, DOE can be used as an auxiliary tool during the optimization step, in order to identify and optimize the significant factors and accomplish competent results through limited experimental trials. In addition, DOE can be divided into screening and optimization designs. In the screening design step, many factors are screened to identify those with the most significant effects, the main designs employed in analytical applications being full factorial, fractional factorial, and Plackett-Burman. While for optimization, response surface designs are used to find the optimal conditions for the most important factors. Among the designs most used are central composite, Box-Behnken, and Doehlert.
O início da produção da cachaça remete ao Ciclo do Açúcar, com o processo de destilo das sobras d... more O início da produção da cachaça remete ao Ciclo do Açúcar, com o processo de destilo das sobras do melaço fermentado de cana. Quando as Antilhas ampliam a produção do açúcar, ocorre a desvalorização do produto brasileiro, o que da início a destilação direta do caldo fermentado. A diferença de matéria prima em relação ao Rum e das madeiras utilizadas para o envelhecimento da bebida permitem concluir que a cachaça é um produto com raízes genuinamente brasileiras.
Desde o desenvolvimento do Ciclo do Ouro, Paraty mostrou destaque na produção de cachaça, que era... more Desde o desenvolvimento do Ciclo do Ouro, Paraty mostrou destaque na produção de cachaça, que era consumida tanto pelo mercado nacional quanto utilizada no escambo por escravos na África e por ouro nas minas, sendo transportada pela Estrada Real. O transporte era realizado em tonéis de carvalho para fora do país e em tonéis de madeiras nacionais para o mercado local. Com o tempo foi observado que cada tipo de madeira incorporava à cachaça odores e sabores diferenciados. Considerando que a cachaça é produzida da fermentação do caldo, diferente do Rum, que é produzido da fermentação do melaço, e que o envelhecimento em diferentes tipos de madeiras adicionavam características sensoriais e químicas específicas, permitiu estabelecer a Cachaça como um produto genuínamente Brasileiro.
Fungicides are applied from plant development to grape production, transport, and storage. Even a... more Fungicides are applied from plant development to grape production, transport, and storage. Even after fruit processing, residues of these compounds can be present in grape by-products such as wine and juice. In this way, a fast and straightforward method based on solvent demulsification-dispersive liquid-liquid microextraction (SD-DLLME) sample preparation was developed, validated, and applied for the multiresidue determination of 30 fungicides in wine using ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). The evaluated SD-DLLME parameters were agitation types, extraction and dispersive solvent type, extraction and dispersive solvent volume, sample pH, and salt types. Sample preparation using SD-DLLME avoids the centrifugation step. Validation was performed using spiked blank sample and satisfactory results for accuracy, with recoveries ranging from 70 to 117% and precision in terms of relative standard deviation ≤20%, except for three compounds at the lowest spiked level. For most of the compounds, the practical method limits of detection and quantification were 0.03 and 0.1 μg L−1, respectively. The method was successfully applied in commercial wine samples in which several pesticides were found at concentrations ranging from 0.109 to 10.6 μg L−1.
Abstract This chapter describes fundamentals and applications of design of experiments (DOE) empl... more Abstract This chapter describes fundamentals and applications of design of experiments (DOE) employed for the method development of sample preparation using solid phase extraction. During method optimization, the presence of a large number of variables (factors) can become a critical step. Thus, DOE can be used as an auxiliary tool during the optimization step, in order to identify and optimize the significant factors and accomplish competent results through limited experimental trials. In addition, DOE can be divided into screening and optimization designs. In the screening design step, many factors are screened to identify those with the most significant effects, the main designs employed in analytical applications being full factorial, fractional factorial, and Plackett-Burman. While for optimization, response surface designs are used to find the optimal conditions for the most important factors. Among the designs most used are central composite, Box-Behnken, and Doehlert.
O início da produção da cachaça remete ao Ciclo do Açúcar, com o processo de destilo das sobras d... more O início da produção da cachaça remete ao Ciclo do Açúcar, com o processo de destilo das sobras do melaço fermentado de cana. Quando as Antilhas ampliam a produção do açúcar, ocorre a desvalorização do produto brasileiro, o que da início a destilação direta do caldo fermentado. A diferença de matéria prima em relação ao Rum e das madeiras utilizadas para o envelhecimento da bebida permitem concluir que a cachaça é um produto com raízes genuinamente brasileiras.
Desde o desenvolvimento do Ciclo do Ouro, Paraty mostrou destaque na produção de cachaça, que era... more Desde o desenvolvimento do Ciclo do Ouro, Paraty mostrou destaque na produção de cachaça, que era consumida tanto pelo mercado nacional quanto utilizada no escambo por escravos na África e por ouro nas minas, sendo transportada pela Estrada Real. O transporte era realizado em tonéis de carvalho para fora do país e em tonéis de madeiras nacionais para o mercado local. Com o tempo foi observado que cada tipo de madeira incorporava à cachaça odores e sabores diferenciados. Considerando que a cachaça é produzida da fermentação do caldo, diferente do Rum, que é produzido da fermentação do melaço, e que o envelhecimento em diferentes tipos de madeiras adicionavam características sensoriais e químicas específicas, permitiu estabelecer a Cachaça como um produto genuínamente Brasileiro.
Fungicides are applied from plant development to grape production, transport, and storage. Even a... more Fungicides are applied from plant development to grape production, transport, and storage. Even after fruit processing, residues of these compounds can be present in grape by-products such as wine and juice. In this way, a fast and straightforward method based on solvent demulsification-dispersive liquid-liquid microextraction (SD-DLLME) sample preparation was developed, validated, and applied for the multiresidue determination of 30 fungicides in wine using ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). The evaluated SD-DLLME parameters were agitation types, extraction and dispersive solvent type, extraction and dispersive solvent volume, sample pH, and salt types. Sample preparation using SD-DLLME avoids the centrifugation step. Validation was performed using spiked blank sample and satisfactory results for accuracy, with recoveries ranging from 70 to 117% and precision in terms of relative standard deviation ≤20%, except for three compounds at the lowest spiked level. For most of the compounds, the practical method limits of detection and quantification were 0.03 and 0.1 μg L−1, respectively. The method was successfully applied in commercial wine samples in which several pesticides were found at concentrations ranging from 0.109 to 10.6 μg L−1.
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