Ultrasound-assisted extraction of azadirachtin from dried entire fruits of Azadirachta indica A. Juss. (Meliaceae) and its determination by a validated HPLC-PDA method
Autor: | Leonardo Luiz Borges, Edemilson Cardoso da Conceição, Karen Lorena Ferreira Neves Caetano, Mariana Cristina de Morais Rodrigues, Lucas Ferreira Brito, Joelma Abadia Marciano de Paula |
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Rok vydání: | 2016 |
Předmět: |
Limonins
Dried fruit Limonoid 01 natural sciences High-performance liquid chromatography Analytical Chemistry chemistry.chemical_compound Limit of Detection medicine Response surface methodology Tetranortriterpenoid Chromatography High Pressure Liquid Azadirachta Meliaceae Chromatography Ethanol biology 010405 organic chemistry 010401 analytical chemistry Temperature Reproducibility of Results biology.organism_classification 0104 chemical sciences Azadirachtin Ultrasonic Waves chemistry Fruit medicine.drug |
Zdroj: | Talanta. 149:77-84 |
ISSN: | 0039-9140 |
DOI: | 10.1016/j.talanta.2015.11.005 |
Popis: | Azadirachta indica A. Juss., also known as neem, is a Meliaceae family tree from India. It is globally known for the insecticidal properties of its limonoid tetranortriterpenoid derivatives, such as azadirachtin. This work aimed to optimize the azadirachtin ultrasound-assisted extraction (UAE) and validate the HPLC-PDA analytical method for the measurement of this marker in neem dried fruit extracts. Box-Behnken design and response surface methodology (RSM) were used to investigate the effect of process variables on the UAE. Three independent variables, including ethanol concentration (%, w/w), temperature (°C), and material-to-solvent ratio (gmL(-1)), were studied. The azadirachtin content (µgmL(-1)), i.e., dependent variable, was quantified by the HPLC-PDA analytical method. Isocratic reversed-phase chromatography was performed using acetonitrile/water (40:60), a flow of 1.0mLmin(-1), detection at 214nm, and C18 column (250×4.6mm(2), 5µm). The primary validation parameters were determined according to ICH guidelines and Brazilian legislation. The results demonstrated that the optimal UAE condition was obtained with ethanol concentration range of 75-80% (w/w), temperature of 30°C, and material-to-solvent ratio of 0.55gmL(-1). The HPLC-PDA analytical method proved to be simple, selective, linear, precise, accurate and robust. The experimental values of azadirachtin content under optimal UAE conditions were in good agreement with the RSM predicted values and were superior to the azadirachtin content of percolated extract. Such findings suggest that UAE is a more efficient extractive process in addition to being simple, fast, and inexpensive. |
Databáze: | OpenAIRE |
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