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药用植物中黄曲霉毒素B1的测定:实验室间研究

Determination of aflatoxin B1 in medical herbs: interlaboratory study.

作者信息

Arranz Isabel, Sizoo Eric, van Egmond Hans, Kroeger Katy, Legarda Teresa M, Burdaspal Pedro, Reif Klaus, Stroka Joerg

机构信息

Institute for Reference Materials and Measurements, Retieseweg 111, B-2440 Geel, Belgium.

出版信息

J AOAC Int. 2006 May-Jun;89(3):595-605.

Abstract

A method was developed for the determination of aflatoxin B1 in medical herbs (senna pods, botanical name Cassia angustifolia; devil's claw, botanical name Harpagophytum procumbens; and ginger roots, botanical name Zingiber officinale). The method, which was tested in a mini-collaborative study by 4 laboratories, is based on an immunoaffinity cleanup followed by reversed-phase high-performance liquid chromatography separation and fluorescence detection after post-column derivatization. It allows the quantitation of aflatoxin B1 at levels lower than 2 ng/g. A second extractant (acetone-water) was tested and compared to the proposed methanol-water extractant. Several post-column derivatization options (electrochemically generated bromine, photochemical reaction, and chemical bromination) as well as different integration modes (height versus area) were also investigated. No differences were found depending on the choice of derivatization system or the signal integration mode used. The method was tested for 3 different matrixes: senna pods, ginger root, and devil's claw. Performance characteristics were established from the results of the study and resulted in HorRat values ranging from 0.12 to 0.75 with mean recoveries from 78 to 91% for the extraction with methanol-water and HorRat values ranging from 0.10-1.03 with mean recoveries from 98 to 103% for the extraction with acetone-water. As a result, the method, with all tested variations, was found to be fit-for-purpose for the determination of aflatoxin B1 in medical herbs at levels of 1 microg/kg and above.

摘要

已开发出一种用于测定草药(番泻豆荚,植物学名狭叶番泻;魔鬼爪,植物学名平卧钩果草;以及姜根,植物学名姜)中黄曲霉毒素B1的方法。该方法经4个实验室的小型协作研究测试,基于免疫亲和净化,随后进行反相高效液相色谱分离,并在柱后衍生化后进行荧光检测。它能够定量测定低于2 ng/g水平的黄曲霉毒素B1。测试了第二种萃取剂(丙酮 - 水)并与提议的甲醇 - 水萃取剂进行比较。还研究了几种柱后衍生化选项(电化学产生溴、光化学反应和化学溴化)以及不同的积分模式(峰高与峰面积)。根据所使用的衍生化系统或信号积分模式的选择未发现差异。该方法针对3种不同基质进行了测试:番泻豆荚、姜根和魔鬼爪。根据研究结果确定了性能特征,甲醇 - 水萃取时HorRat值范围为0.12至0.75,平均回收率为78%至91%;丙酮 - 水萃取时HorRat值范围为0.10至1.03,平均回收率为98%至103%。结果表明,该方法及其所有测试变体适用于测定含量为1μg/kg及以上的草药中的黄曲霉毒素B1。

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