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目的建立玉米等谷物中玉米赤霉烯酮测定的高效液相色谱法。方法样品用乙腈提取,50℃氮吹干,乙腈定容后进样色谱分析。色谱条件:分离柱为Hypersil C_(18)(250 mm×4.6 mm,5μm);流动相为甲醇-0.02 mol/L乙酸铵(70∶30,V/V);检测波长为236 nm。结果本法在0μg/ml~10μg/ml条件下,线性关系良好(r=0.999 95),ZEN的回归方程为y=81.25x+1.64,方法的检出限为5.0μg/kg。对玉米、小麦、稻谷3类样品分别作了低、中、高3种浓度的加标回收实验,回收率为84.0%~112%,相对标准偏差(RSD)为2.9%~7.1%。结论本法样品处理简单,操作方便,灵敏度高、稳定性好、成本低,可作为谷物中玉米赤霉烯酮定量测定的有效手段。
Objective To establish a method for the determination of zearalenone in corn and other grains by high performance liquid chromatography. Methods The samples were extracted with acetonitrile, dried by nitrogen at 50 ℃, and injected into the chromatographic column. Chromatographic conditions: the separation column was Hypersil C18 (250 mm × 4.6 mm, 5 μm); the mobile phase was methanol-0.02 mol / L ammonium acetate (70:30, V / V); the detection wavelength was 236 nm. Results The linear relationship was good (r = 0.999 95) at 0μg / ml ~ 10μg / ml. The regression equation of ZEN was y = 81.25x + 1.64. The detection limit was 5.0μg / kg. The spiked recoveries of three kinds of maize, wheat and rice at low, medium and high concentrations were obtained. The recovery rates ranged from 84.0% to 112% and the relative standard deviations (RSDs) ranged from 2.9% to 7.1%. Conclusion The sample of this method has the advantages of simple processing, convenient operation, high sensitivity, good stability and low cost and can be used as an effective method for the quantitative determination of zearalenone in cereals.