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玉米中α-玉米赤霉醇和玉米赤霉烯酮的液相色谱测定:协同研究

Liquid chromatographic determination of alpha-zearalenol and zearalenone in corn: collaborative study.

作者信息

Bennett G A, Shotwell O L, Kwolek W F

出版信息

J Assoc Off Anal Chem. 1985 Sep-Oct;68(5):958-61.

PMID:2932426
Abstract

The liquid chromatographic determination of alpha-zearalenol and zearalenone in corn was collaboratively studied. Each of 13 collaborators received 7 corn samples; 2 were blanks and 5 were spiked to contain 50, 100, and 200 ng alpha-zearalenol/g and 50, 100, 500, 1000, and 4000 ng zearalenone/g. Four sets (including blanks) of blind duplicates were included in the study. Five naturally contaminated corn samples (one in duplicate) were also provided. All collaborators detected both mycotoxins at 50 ng/g. Average recoveries reported by all collaborators ranged from 81.9% at 200 ng/g to 100.3% at 50 ng/g for alpha-zearalenol and from 77.8% at 1000 ng/g to 123% at 50 ng/g for zearalenone. Three collaborators reported false positives for both alpha-zearalenol and zearalenone. The within-laboratory CV values based on blind duplicates were 22.6% for alpha-zearalenol and 31.4% for zearalenone. The CV values based on laboratory-sample interaction were 25.6 and 33.8% for alpha-zearalenol and zearalenone, respectively. The CV values for naturally contaminated samples (including duplicates) were 47.0% for alpha-zearalenol and 37.7% for zearalenone. The method has been adopted official first action.

摘要

对玉米中α-玉米赤霉醇和玉米赤霉烯酮的液相色谱测定方法进行了协同研究。13位协作人员每人收到7个玉米样品;其中2个为空白样,5个为加标样,分别含有50、100和200 ng/g的α-玉米赤霉醇以及50、100、500、1000和4000 ng/g的玉米赤霉烯酮。该研究包括四组(含空白样)盲法双样。还提供了5个天然污染的玉米样品(其中1个为双份)。所有协作人员均能检测出50 ng/g的两种霉菌毒素。所有协作人员报告的平均回收率,α-玉米赤霉醇在200 ng/g时为81.9%,在50 ng/g时为100.3%;玉米赤霉烯酮在1000 ng/g时为77.8%,在50 ng/g时为123%。有3位协作人员报告了α-玉米赤霉醇和玉米赤霉烯酮的假阳性结果。基于盲法双样的实验室内变异系数(CV)值,α-玉米赤霉醇为22.6%,玉米赤霉烯酮为31.4%。基于实验室与样品相互作用的CV值,α-玉米赤霉醇和玉米赤霉烯酮分别为25.6%和33.8%。天然污染样品(包括双份样)的CV值,α-玉米赤霉醇为47.0%,玉米赤霉烯酮为37.7%。该方法已被采用为官方首次行动方法。

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