研究了高效液相色谱法测定玉米中玉米赤霉烯酮的方法。样品借鉴了GB/T 19540-2004中提取玉米赤霉烯酮的方法,通过Oasis HLB净化柱对提取液净化,以agilent extent C18色谱柱为分离柱,乙腈-水(V水∶V乙腈=55∶45)为流动相进行荧光检测(λex=235 nm,λem=460 nm)。玉米赤霉烯酮的质量浓度在12—2 400μg/kg范围内呈良好线性,相关系数为0.9994,对添加高、中、低3个浓度玉米赤霉烯酮的玉米样品进行加标回收试验,平均回收率分别为96.736%、93.839%、86.240%,变异系数在1%—10%之间,最低检测限为10μg/kg。此方法对玉米中玉米赤霉烯酮的检测是可行的,且可给谷物中玉米赤霉烯酮检测方法优化提供参考。
A method was established for determination of mycotoxin zearalenone(ZEN) in maize by high performance liquid chromatography(HPLC). Using the method of GB/T 19540:2004 as reference, samples were cleaned up through Oasis HLB column. Extracted samples were analyzed by HPLC on an agilent extent C18 column with acetonitrile/water (45 :55) as mobile phase (1.0 mL min 1), and fluorescence detection (λex = 235 nm,λem = 460 nm) was conducted. Resuits: The calibration graphs are linear up from 12 - 2 400μg/kg for ZEN in maize and correlation coefficient is 0.9994. For maize samples added with high, middle or low level of ZEN reference material, the recovery is 86.240%, 93. 839%, 96.736%, respectively. The relative standard deviations are 1% - 10%, and the minimum detection limit is 10μg/kg. This determination method for ZEN is feasible and may also provide reference to improve ZEN determination in other cereal grains.