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谷物中镰刀菌霉菌毒素串珠镰刀菌素的液相色谱测定及稳定性

Liquid chromatographic determination and stability of the Fusarium mycotoxin moniliformin in cereal grains.

作者信息

Scott P M, Lawrence G A

机构信息

Health and Welfare Canada, Food Research Division, Ottawa, Ontario.

出版信息

J Assoc Off Anal Chem. 1987 Sep-Oct;70(5):850-3.

PMID:3680124
Abstract

Moniliformin is a mycotoxin produced by Fusarium subglutinans and other Fusarium species. A rapid, liquid chromatographic method for its determination in corn and wheat is described. Samples are extracted in acetonitrile-water (95 + 5); following defatting with n-hexane, an aliquot of the extract is evaporated and cleaned up on small C18 and neutral alumina columns successively. Reverse-phase liquid chromatography (LC) is conducted on a C18 column with 10 or 15% methanol or acetonitrile in aqueous ion-pair reagent as mobile phase, with detection by ultraviolet absorption at 229 and 254 nm. Average recoveries of moniliformin (potassium salt) added to ground corn and wheat at levels of 0.05-1.0 micrograms/g were 80% (n = 20) and 85% (n = 12), respectively, and the limit of detection was ca 0.01-0.18 micrograms/g, depending on LC conditions. Analysis of 24 samples of wheat, 4 samples of rye, and 12 samples of corn showed moniliformin in only 2 corn samples (0.06 and 0.2 micrograms/g). Moniliformin was also detected in a sample of artificially damaged (slashed) corn (0.2 micrograms/g) and selected kernels of corn that were field-inoculated with F. subglutinans and F. moniliforme (50 micrograms/g and 0.5 micrograms/g, respectively). In stability studies, moniliformin (potassium salt, 1 microgram/g) in ground corn and ground wheat heated at 50, 100, and 150 degrees C for 0.5-2 h decomposed moderately, e.g., 55% remained in corn after 0.5 h at 100 degrees C.

摘要

串珠镰刀菌素是由亚粘团镰刀菌和其他镰刀菌属物种产生的一种霉菌毒素。本文描述了一种用于测定玉米和小麦中该毒素的快速液相色谱法。样品用乙腈 - 水(95 + 5)提取;用正己烷脱脂后,取一部分提取物蒸发,并先后在小的C18柱和中性氧化铝柱上进行净化。反相液相色谱(LC)在C18柱上进行,以含10%或15%甲醇或乙腈的水性离子对试剂作为流动相,通过在229和254 nm处的紫外吸收进行检测。添加到磨碎玉米和小麦中水平为0.05 - 1.0微克/克的串珠镰刀菌素(钾盐)的平均回收率分别为80%(n = 20)和85%(n = 12),检测限约为0.01 - 0.18微克/克,具体取决于液相色谱条件。对24个小麦样品、4个黑麦样品和12个玉米样品的分析表明,仅在2个玉米样品中检测到串珠镰刀菌素(0.06和0.2微克/克)。在一个人工损伤(划破)的玉米样品(0.2微克/克)以及用亚粘团镰刀菌和串珠镰刀菌进行田间接种的选定玉米籽粒(分别为50微克/克和0.5微克/克)中也检测到了串珠镰刀菌素。在稳定性研究中,磨碎玉米和磨碎小麦中1微克/克的串珠镰刀菌素(钾盐)在50、100和150℃加热0.5 - 2小时后会适度分解,例如,在100℃加热0.5小时后,玉米中仍残留55%。

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