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使用萃取盘分离α-玉米赤霉醇和玉米赤霉烯酮的制备方法。

Preparative method for isolating alpha-zearalenol and zearalenone using extracting disk.

作者信息

Ware G M, Zhao Y, Kuan S S, Carman A S

机构信息

U.S. Food and Drug Administration, Natural Toxins Research Center, New Orleans, LA 70122, USA.

出版信息

J AOAC Int. 1999 Jan-Feb;82(1):90-4.

PMID:10028676
Abstract

A liquid chromatographic method is described for the determination of zearalenol and zearalenone in corn. Zearalenol and zearalenone are extracted from corn with methanol-water (1 + 1) and cleaned up using a solid-phase extraction (SPE) disk, separated on a reversed-phase analytical column, and detected with a fluorescence detector. The SPE disk concentrated and cleanly separated zearalenol and zearalenone from sample interferences. Standard calibration curves for zearalenol and zearalenone for the concentration range 25-500 ng/mL were linear. The small extract disk had a column capacity equivalent to 1 g extracted corn. Zearalenol and zearalenone were added at levels ranging from 10 to 2000 ng/g to a control sample that contained no detectable levels of zearalenol and zearalenone. Both toxins were recovered from spiked samples at 106.3 and 103.8%, with coefficients of variation of 7.6 and 13.0%, respectively. The method has an estimated reliable limit of detection and limit of quantitation around 10 and 40 ng/g for each toxin, respectively.

摘要

描述了一种用于测定玉米中玉米赤霉烯醇和玉米赤霉酮的液相色谱方法。玉米赤霉烯醇和玉米赤霉酮用甲醇 - 水(1 + 1)从玉米中提取,并用固相萃取(SPE)盘净化,在反相分析柱上分离,并用荧光检测器检测。SPE盘将玉米赤霉烯醇和玉米赤霉酮与样品干扰物浓缩并干净地分离。玉米赤霉烯醇和玉米赤霉酮在25 - 500 ng/mL浓度范围内的标准校准曲线呈线性。小萃取盘的柱容量相当于1 g提取的玉米。将玉米赤霉烯醇和玉米赤霉酮以10至2000 ng/g的水平添加到不含可检测水平的玉米赤霉烯醇和玉米赤霉酮的对照样品中。两种毒素在加标样品中的回收率分别为106.3%和103.8%,变异系数分别为7.6%和13.0%。该方法估计每种毒素的可靠检测限和定量限分别约为10和40 ng/g。

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