玉米制品中黄曲霉毒素的柱前和柱后衍生方法对比

Comparison of Pre-column Derivatization and Post-column Derivatizationfor Aflatoxin in Corn Products

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Mycrosep ^(TM)226多功能净化柱净化,采用Waters Symmetry C18(4.6 mm×250 mm,5.0μm)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G_1、B_1检出限为0.05μg/kg,黄曲霉毒素G_2、B_2检出限为0.015μg/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G_1、B_1检出限为0.08μg/kg,黄曲霉毒素G_2、B_2检出限为0.015μg/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。

To compare 2 derivatization methods for determination of aflatoxin in corn products（pre-column derivatization and post-column derivatization）.The samples were purified by Mycrosep ^TM 226 multifunction purification column,separated by Waters Symmetry C18（4.6 mm×250 mm,5.0 μm）and the fluorescence detector 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 extract 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 was0.015 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.