一种测定谷物制品中玉米赤霉烯酮的 HPTLC 方法。

A HPTLC method for the determination of the mycotoxin zearalenone in cereal products.

机构信息

National Institute of Public Health Prague, Centre for the Hygiene of Food Chains in Brno, National Reference Centre for Microscopic Fungi and Mycotoxins in Food Chains, The Czech Republic,

出版信息

Mycotoxin Res. 2003 Mar;19(1):64-8. doi: 10.1007/BF02940096.

DOI:10.1007/BF02940096

PMID:23604672

Abstract

An HPTLC method for the quantification of zearalenone (ZEA) in cereals and cereal products (wheat flour and malt) has been developed. ZEA was extracted with 50 ml of acetonitrile-purified water (9+1) with addition of 2 g NaCl. The extracts were further purified on VICAM ZearalaTest((tm)) immunoaffinity columns, then analysed by instrumental high-performance thin-layer chromatography (HPTLC) on silica gel plates with fluorescence detection. Ethyl acetate - n-hexane (1+1) was used as the mobile phase. The chromatogram was scanned in fluorescence mode after excitation at λ=254 nm with λ=400 nm measuring filter: SENS and SPAN parameters were 195 and 20, respectively. TheR F of ZEA under these conditions was 0.43.The recovery was 95% in the range 15-65 µg/kg cereal products; the mean relative standard deviation of repeatability (RSDr) was 7.6%. The limit of quantification (LoQ) of ZEA was 10 µg/kg. Validation of the method was performed according to the principles of the ICH for pharmaceutical analysis.

摘要

建立了一种用于谷物和谷物制品（小麦粉和麦芽）中玉米赤霉烯酮（ZEA）定量的 HPTLC 方法。ZEA 用 50ml 乙腈-纯水（9+1）提取，加入 2g NaCl。提取物进一步用 VICAM ZearalaTest（tm）免疫亲和柱纯化，然后用硅胶板进行仪器高效薄层色谱（HPTLC）分析，荧光检测。乙酸乙酯-正己烷（1+1）为流动相。在 254nm 激发波长和 400nm 测量滤光片下，以荧光模式扫描色谱图：SENS 和 SPAN 参数分别为 195 和 20。在此条件下，ZEA 的 RF 值为 0.43。谷物制品中 ZEA 的回收率在 15-65μg/kg 范围内为 95%；重复性（RSDr）的平均相对标准偏差为 7.6%。ZEA 的定量限（LoQ）为 10μg/kg。该方法的验证按照制药分析 ICH 的原则进行。