麦类中玉米赤霉烯酮的快速检测

Rapid Determination of Zearalenone in Wheat

提出了高效液相色谱荧光检测法测定麦类样品中玉米赤霉烯酮的方法。样品经乙腈-水(84+16,体积比)提取,多功能柱净化,C_(18)色谱柱(4.6 mm×250 mm,5μm)分离,水-乙腈-甲醇(46+46+8,体积比)混合溶液作流动相,流速1.0 mL·min^(-1)。玉米赤霉烯酮的质量浓度在20.0～5 000μg·L^(-1)范围内,峰面积与玉米赤霉烯酮浓度之间呈线性关系,样品在50.0,100.0,1 000.0 ng·g^(-1)添加水平的平均回收率分别为74.6%,75.5%,73.5%,相对标准偏差为9.7%～11.5%(n=8)之间,方法的测定限(10S/N)为50.0 ng·g^(-1)。

HPLC with fluorescence emission intensity detection was used in the determination of zearalenone in wheat. Zearalenone was separated from the sample by extraction with a mixed solvent ot acetonltrne anu warer （mixed in the vol. ratio of 84 to 16）, and the extract was purified by passing through the muhifunctional column. Chromatographic separation was carried out on the C18 column （4. 6 mm×250 mm, 5 μm） and eluted with a mixture containing water, acetonitrile and methanol （mixed in the vol. ratio of 46 to 46 to 8）, flowing at a rate of 1.0 mL · min^-1. Linear relationship between values of peak area and concentration of zearalenone was obtained in the range of 20. 0 to 5 000. 0 μg · L^-1. Tests for recovery and precision were made at the concentration levels of 50. 0, 100. 0 and 1 000.0 ng · g^-1 , and values of average recovery 74. 6%, 75. 5%, 73. 5%, and values of RSD＇ s （n = 8） calculated were in the range of 9.7%- 11. 5%. Lower limit of determination （10S/N） of the method found was 50. 0 ng · g^-1.