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食品研究与开发:2017,38(14):144-146
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玉米制品中黄曲霉毒素的柱前和柱后衍生方法对比
王敏,李广益,邢燕*,李婷婷,王勤
(淄博市疾病预防控制中心,山东 淄博 255026)
Comparison of Pre-column Derivatization and Post-column Derivatizationfor Aflatoxin in Corn Products
WANG Min, LI Guang-yi, XING Yan*, LI Ting-ting, WANG Qin
(Zibo Center for Disease Control and Prevention, Zibo 255026, Shandong, China)
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投稿时间:2016-10-17    
中文摘要: 玉米制品中黄曲霉毒素测定的 2 种衍生化方法(柱前衍生和柱后衍生)进行比较。 样品经过 MycrosepTM226 多功能净化柱净化,采用 Waters Symmetry C18(4.6 mm×250 mm,5.0 μm)色谱柱进行分离,荧光检测器检测。柱前衍生 法:样品提取液经净化后,采用三氟乙酸进行衍生后测定。柱后碘衍生法:样品提取液经净化后,经高效液相色谱分 离、柱后碘衍生,荧光检测器检测。结果表明:柱前衍生法,黄曲霉毒素 G1、B1 检出限为 0.05 μg/kg,黄曲霉毒素 G2、B2 检出限为 0.015 μg/kg,r>0.999 1,回收率在 75.4 %~84.2 %之间;柱后碘衍生法,黄曲霉毒素 G1、B1 检出限为 0.08 μg/kg, 黄曲霉毒素 G2、B2 检出限为 0.015 μg/kg,r>0.999 2,回收率在 75.2 %~85.7 %之间。2 种衍生方法在线性范围、精密度、 回收率等方面较相似,表明柱前衍生法和柱后碘衍生法均适用于玉米制品中的黄曲霉毒素检测。
中文关键词: 黄曲霉毒素  柱前衍生  柱后衍生  对比
Abstract:To compare 2 derivatization methods for determination of aflatoxin in corn products (pre-column derivatization and post-column derivatization). The samples were purified by MycrosepTM 226 multifunction pu- rification column , separated by Waters Symmetry C18 (4.6 mm×250 mm, 5.0 μm) and the fluorescence de- tector was used. Pre-column derivatizationmethod:sample extraction solution was determined by the use of three fluorine acetic acid for derivatization after purification. Post-column derivatization with iodine:the sample ex- tract was purified by high performance liquid chromatography, and then detected by fluorescence detector. For pre-column derivatization, the detection limit of aflatoxin G1, B1 was 0.05 μg/kg, the detection limit of aflatoxin G2, B2 was 0.015 μg/kg ,r > 0.999 1, and the recovery rate was between 75.4 % and 84.2 %; for post-column derivatization, the detection limit of aflatoxin G1, B1 was 0.08 μg/kg, the detection limit of aflatoxin G2, B2 was 0.015 μg/kg ,r > 0.999 2, and the recovery rate was between 75.2 % and 85.7 %.The 2 methods are similar in terms of linear range, precision, recovery and so on. The results showed that the pre-column derivatization and post-column derivatization are all suitable for the detection of aflatoxin in corn products.
文章编号:201714030     中图分类号:    文献标志码:A
基金项目:山东省自然科学基金项目(ZR2015PH035);山东省医药卫生科技发展计划项目(2013WS0028)
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