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西班牙蜂花粉中黄曲霉毒素和赭曲霉毒素A的免疫亲和柱同时净化及高效液相色谱分析

Simultaneous immunoaffinity column cleanup and HPLC analysis of aflatoxins and ochratoxin A in Spanish bee pollen.

作者信息

Garcia-Villanova Rafael J, Cordón Carlos, González Paramás Ana M, Aparicio P, Garcia Rosales M Eugenia

机构信息

Departamento de Química Analítica, Nutrición y Bromatología, Facultad de Farmacia, Universidad de Salamanca, Campus Miguel de Unamuno, E-37007 Salamanca, Spain.

出版信息

J Agric Food Chem. 2004 Dec 1;52(24):7235-9. doi: 10.1021/jf048882z.

DOI:10.1021/jf048882z
PMID:15563200
Abstract

Bee pollen is a major substrate for mycotoxins growth when no prompt and adequate drying is performed by the beekeeper after collection by bees. Regulatory limits for aflatoxins and ochratoxin A are currently in force in the European Union for a rising list of foodstuffs, but not for this. An immunoaffinity column cleanup process has been applied prior to the analysis of aflatoxins B(1), B(2), G(1), and G(2) and ochratoxin A (OTA). Optimization of the HPLC conditions has involved both a gradient elution and a wavelength program for the separation and fluorimetric quantitation of all five mycotoxins at their maximum excitation and emission values of wavelength in a single run. The higher limit of detection (mug/kg) was 0.49 for OTA and 0.20 for aflatoxin B(1). Repeatability (RSDr) at the lower limit tested ranged from 9.85% for OTA to 6.23% for aflatoxin G(2), and recoveries also at the lower spiked level were 73% for OTA and 81% for aflatoxin B(1). None of the 20 samples assayed showed quantifiable values for the five mycotoxins.

摘要

如果养蜂人在蜜蜂采集后没有及时进行充分干燥,蜂花粉就会成为霉菌毒素生长的主要基质。目前欧盟对越来越多的食品实施了黄曲霉毒素和赭曲霉毒素A的监管限量,但对蜂花粉没有。在分析黄曲霉毒素B(1)、B(2)、G(1)和G(2)以及赭曲霉毒素A(OTA)之前,采用了免疫亲和柱净化程序。高效液相色谱条件的优化包括梯度洗脱和波长程序,以便在一次运行中以所有五种霉菌毒素的最大激发和发射波长值进行分离和荧光定量。OTA的检测上限(μg/kg)为0.49,黄曲霉毒素B(1)为0.20。在测试的下限处,重复性(RSDr)范围从OTA的9.85%到黄曲霉毒素G(2)的6.23%,在较低加标水平下,OTA的回收率为73%,黄曲霉毒素B(1)为81%。所检测的20个样品中,没有一个显示出这五种霉菌毒素的可量化值。

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