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液质联用技术同时检测霉变谷物中玉米赤霉醇及其代谢物和玉米赤霉烯酮的方法

Liquid chromatography incorporating ultraviolet and electrochemical analyses for dual detection of zeranol and zearalenone metabolites in mouldy grains.

机构信息

Department of Veterinary Medicine, College of Veterinary Medicine, National Chung-Hsing University, Taichung 402, Taiwan.

出版信息

J Sci Food Agric. 2012 Apr;92(6):1230-7. doi: 10.1002/jsfa.4687. Epub 2011 Oct 19.

Abstract

BACKGROUND

Zeranol (Z) is a semi-synthetic mycotoxin that is used in some countries as a growth-promoting agent in livestock. In view of the known oestrogenic actions by Z and certain Z analogues, significant concerns exist with regard to the presence of Z residues in human foods and the potential for untoward effects, including carcinogenicity within the reproductive system. In order to confirm that foods are free from harmful Z residues, regulators need a quick and reliable analytical method that can be used for routine confirmation of Z-positive samples identified by enzyme-linked immunosorbent assay (ELISA) screening. In this study the authors have developed and validated a simple and rapid high-performance liquid chromatography method incorporating ultraviolet (UV) absorbance (wavelength 274 nm) and electrochemical (EC) dual-mode detection for simultaneous determination of Z-related mycotoxins produced from mouldy grain matrices, including rice, soybean and corn flakes.

RESULTS

Recoveries for all analytes were around 80% and the limits of detection ranged from 10 to 25 ng mL(-1) for UV and from 50 to 90 ng mL(-1) for EC detection with good accuracy and reproducibility. Differential profiles and occurrence rates of Z, β-zearalenol, β-zearalanol and α-zearalenol in naturally moulded grain matrices were observed, indicating different metabolite patterns and possibly grain-specific effects of mycotoxin exposure for humans and animals. The strength of this dual detection method lies in its selectivity characterised by a carbon screen-printed electrode such that aflatoxin interference is precluded.

CONCLUSION

The combined dual detection technique affords quick and reliable semi-confirmative and quantitative information on multiple types of Z analogues in mouldy grains without the necessity of using expensive mass spectrometry. The method is considered a superior supplement to ELISA, which only screens total Z immunoreactivity.

摘要

背景

泽仑诺(Z)是一种半合成霉菌毒素,在一些国家被用作牲畜的生长促进剂。鉴于 Z 和某些 Z 类似物具有已知的雌激素作用,人们对人类食品中存在 Z 残留以及潜在的不良影响(包括生殖系统的致癌性)表示严重关切。为了确认食品中没有有害的 Z 残留,监管机构需要一种快速可靠的分析方法,用于对酶联免疫吸附测定(ELISA)筛选确定的 Z 阳性样品进行常规确认。在这项研究中,作者开发并验证了一种简单快速的高效液相色谱法,该方法结合了紫外(UV)吸收(波长 274nm)和电化学(EC)双模式检测,可同时测定来自霉变谷物基质(包括大米、大豆和玉米片)的 Z 相关霉菌毒素。

结果

所有分析物的回收率约为 80%,UV 检测的检出限范围为 10 至 25ng/mL,EC 检测的检出限范围为 50 至 90ng/mL,具有良好的准确性和重现性。在天然霉变谷物基质中观察到 Z、β-玉米赤霉醇、β-玉米赤霉烯醇和α-玉米赤霉烯醇的差异图谱和出现率,表明存在不同的代谢物图谱,可能对人和动物的霉菌毒素暴露具有谷物特异性影响。这种双检测方法的优势在于其选择性,这得益于碳印刷电极,可排除黄曲霉毒素的干扰。

结论

该联合双检测技术可快速可靠地提供关于霉变谷物中多种类型 Z 类似物的半确证和定量信息,而无需使用昂贵的质谱法。该方法被认为是 ELISA 的一种优越补充,ELISA 仅筛选总 Z 免疫反应性。

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