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首页> 外文期刊>Brazilian Journal of Microbiology >Intralaboratory optimization and validation of a method for patulin determination in grapes by Thin-Layer Chromatography
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Intralaboratory optimization and validation of a method for patulin determination in grapes by Thin-Layer Chromatography

机译：实验室内优化和薄层色谱法测定葡萄中棒曲霉素的方法的验证

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摘要

The aim of this work was to optimize and validate, by intralaboratorial procedures, a method for the determination of patulin in grapes by thin-layer chromatography. The steps of extraction, cleanup, detection and quantification were optimized. For the validation of the method, recovery assays with standard solutions and artificially contaminated samples were carried out. The mean recovery and the variation coefficient were 65.4% and 7.58%, respectively. The optimized conditions were: 50 mL of grape juice, three extraction stages (with 100 mL of ethyl acetate in the first stage and 50 mL in second and third stages), and 100 μL of ethanol to solubilize the extract. The solvent-system used was toluene - ethyl acetate - formic acid (6:3:1), and 0.5% MBTH in 5% formic acid was sprayed on the plates to intensify the fluorescence. The visual detection and quantification limits were 7.44 ng and 15.87 μg.kg-1, respectively. The optimized and validated method demonstrated sufficient efficiency for adoption in the monitoring of patulin in grape.
机译：这项工作的目的是通过实验室内部程序优化和验证一种通过薄层色谱法测定葡萄中棒曲霉素的方法。优化了提取，纯化，检测和定量步骤。为了验证该方法，使用标准溶液和人工污染的样品进行了回收率测定。平均回收率和变异系数分别为65.4％和7.58％。优化的条件是：50 mL葡萄汁，三个提取阶段（第一阶段使用100 mL乙酸乙酯，第二阶段和第三阶段使用50 mL）和100μL乙醇使提取物增溶。所使用的溶剂系统是甲苯-乙酸​​乙酯-甲酸（6：3：1），并将在5％甲酸中的0.5％MBTH喷涂在板上以增强荧光。视觉检测和定量限分别为7.44 ng和15.87μg.kg-1。经过优化和验证的方法显示出足够的效率，可用于监测葡萄中的棒曲霉素。

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