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免疫亲和柱结合液相色谱法测定罐装和冷冻甜玉米中的伏马毒素B1

Immunoaffinity column coupled with liquid chromatography for determination of fumonisin B1 in canned and frozen sweet corn.

作者信息

Trucksess M W, Stack M E, Allen S, Barrion N

机构信息

U.S. Food and Drug Administration, Division of Natural Products, Washington, DC 20204, USA.

出版信息

J AOAC Int. 1995 May-Jun;78(3):705-10.

PMID:7756885
Abstract

A modified liquid chromatographic (LC) method for determining fumonisin B1 (FB1) in corn was applied to canned and frozen sweet corn. The corn is extracted with methanol-water (8 + 2), and the extract is filtered. The filtrate is diluted with water and passed through an immunoaffinity column. After the column is washed with water, FB1 is eluted with methanol-water (8 + 2). The eluate is evaporated to dryness by using a vacuum concentrator, and the residue is dissolved in acetonitrile-water (1 + 1). FB1 is derivatized with o-phthaldialdehyde. The derivative is separated on a reversed-phase C18 LC column using acetonitrile-water-acetic acid (50 + 50 + 1) and quantitated with a fluorescence detector. Recoveries of FB1 from canned and frozen corn spiked over the range of 50-200 ng/g were 76-88%. The limit of determination was about 25 ng/g, and the limit of detection was about 4 ng/g. The method was applied to 97 commercial canned and frozen sweet corn samples collected from different areas of the United States. Sixty samples contained no FB1. Low levels (trace-82 ng FB1/g corn) were found in 35 samples; 235 ng FB1/g was found in 1 canned corn sample, and 350 ng FB1/g was found in 1 frozen corn sample.

摘要

一种用于测定玉米中伏马菌素B1(FB1)的改良液相色谱(LC)方法被应用于罐装和冷冻甜玉米。玉米用甲醇-水(8 + 2)提取,提取物过滤。滤液用水稀释并通过免疫亲和柱。柱用水洗涤后,FB1用甲醇-水(8 + 2)洗脱。洗脱液用真空浓缩器蒸发至干,残留物溶于乙腈-水(1 + 1)。FB1用邻苯二甲醛衍生化。衍生物在反相C18液相色谱柱上用乙腈-水-乙酸(50 + 50 + 1)分离,并用荧光检测器定量。在添加量为50 - 200 ng/g范围内的罐装和冷冻玉米中FB1的回收率为76 - 88%。测定限约为25 ng/g,检测限约为4 ng/g。该方法应用于从美国不同地区收集的97个商业罐装和冷冻甜玉米样品。60个样品未含FB1。35个样品中发现低水平(痕量 - 82 ng FB1/g玉米);1个罐装玉米样品中发现235 ng FB1/g,1个冷冻玉米样品中发现350 ng FB1/g。

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