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谷物中脱氧雪腐镰刀菌烯醇的一步固相萃取净化及荧光分析

One-step solid-phase extraction cleanup and fluorometric analysis of deoxynivalenol in grains.

作者信息

Malone B R, Humphrey C W, Romer T R, Richard J L

机构信息

Romer Labs, Inc., Union, MO 63084, USA.

出版信息

J AOAC Int. 1998 Mar-Apr;81(2):448-52.

PMID:9549079
Abstract

A rapid, quantitative, inexpensive, efficient method was developed to determine deoxynivalenol (DON) in wheat, barley, corn, wheat middlings, wheat flour, bran, malted barley, and oats. Samples are ground and extracted with acetonitrile-water (86 + 14). A portion of the extract is cleaned up by passage through a MycoSep No. 225 column, evaporated to dryness, and derivatized with zirconyl nitrate and ethylenediamine in methanol. The resulting fluorescent derivative of DON is identified and quantitated with a calibrated fluorometer containing a broad wavelength pulsed xenon light source. This method quantitated DON concentrations from 0.5 to 50 ppm without dilution and was linear when applied to samples of noncontaminated wheat spiked at 0.5, 5, 10, 25, and 50 micrograms DON/g. Correlation coefficients of the method with LC for multiple analyses (n > or = 14 for each commodity) applied to wheat, corn, barley, wheat flour, and wheat middlings were 0.99, 0.99, 0.99, 0.93, and 0.98, respectively. Individual analyses were conducted in < 30 min, and 24 samples were analyzed in 2 h.

摘要

开发了一种快速、定量、廉价、高效的方法来测定小麦、大麦、玉米、小麦麸、小麦粉、麸皮、麦芽大麦和燕麦中的脱氧雪腐镰刀菌烯醇(DON)。将样品研磨后用乙腈 - 水(86 + 14)提取。取一部分提取物通过MycoSep No. 225柱进行净化,蒸发至干,然后在甲醇中用硝酸锆酰和乙二胺进行衍生化。所得DON的荧光衍生物用含有宽波长脉冲氙光源的校准荧光计进行鉴定和定量。该方法无需稀释即可定量0.5至50 ppm的DON浓度,应用于添加了0.5、5、10、25和50微克DON / g的未受污染小麦样品时呈线性。该方法与液相色谱法对小麦、玉米、大麦、小麦粉和小麦麸进行多次分析(每种商品n≥14)的相关系数分别为0.99、0.99、0.99、0.93和0.98。单个分析在30分钟内完成,2小时内可分析24个样品。

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