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High-throughput modified QuEChERS method for the determination of the mycotoxin tenuazonic acid in wine grapes

机译:高通量改良型QuEChERS方法测定酿酒葡萄中的霉菌毒素Tenuazonic酸

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摘要

A reliable, simple, fast, inexpensive and robust sample preparation approach for tenuazonic acid (TA) determination in grapes by liquid chromatography with ultraviolet detection (HPLC-UV) is proposed. The method is based on a modified QuEChERS (quick, easy, cheap, effective, rugged and safe) approach using ethyl acetate as extraction solvent. Its involves extraction of 2.5 g sample (plus 2.5 mL 1% formic acid acidified water) with 5 mL of ethyl acetate; drying/cleaning- up of extract with 0.25 g anhydrous CaCl2 and determination by HPLC-UV. The method was optimized and validated achieving a limit of quantification (LOQ) of 0.05 mu g g(-1). The overall recoveries were 96%, 82% and 97% for grape samples spiked at 0.05, 0.5 and 5 mu g g(-1), respectively. The method showed excellent reproducibility with RSDs for the above data <= 8% and Horwitz ratios <0.11. The procedure was applied to evaluate the occurrence of TA in grapes and it was quantified at concentrations ranging between 0.057 and 0.595 mu g g(-1). The methodological development allows a high throughput routine quality control of grapes, adding a valuable tool for the winemaking industry. The method could be applied in an average laboratory and help to understand possible effects related to Alternaria rotting on the final wines elaborated. As well, this is the first report of TA presence in grapes used for wine elaboration, so the results add new knowledge to a growing research area.
机译:提出了一种可靠的,简单,快速,廉价且稳定的样品制备方法,用于液相色谱-紫外检测(HPLC-UV)法测定葡萄中的替硝唑酸(TA)。该方法基于改良的QuEChERS(快速,简便,便宜,有效,坚固和安全)方法,使用乙酸乙酯作为萃取溶剂。它涉及用5 mL乙酸乙酯萃取2.5 g样品(加2.5 mL 1%甲酸酸化的水);用0.25 g无水CaCl2干燥/纯化萃取物,并通过HPLC-UV测定。该方法进行了优化和验证,实现了0.05μg g(-1)的定量限(LOQ)。分别以0.05、0.5和5 g g(-1)加标的葡萄样品的总回收率分别为96%,82%和97%。对于上述数据<= 8%和Horwitz比<0.11,该方法对RSD表现出优异的重现性。该程序用于评估葡萄中TA的存在,并在0.057至0.595μg g(-1)范围内对其进行了定量。方法论的发展使葡萄的高通量常规质量控制成为可能,为酿酒业增加了有价值的工具。该方法可在一般实验室中应用,并有助于了解与链格孢菌腐烂有关的最终葡萄酒可能产生的影响。同样,这也是用于葡萄酒酿造的葡萄中TA含量的首次报道,因此研究结果为不断发展的研究领域增加了新的知识。

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