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目的建立小麦和玉米中脱氧雪腐镰刀菌烯醇与雪腐镰刀菌烯醇的免疫亲和净化-高效液相色谱检测方法。方法样品经纯水提取后,用免疫亲和柱净化,经甲醇洗脱,在C18色谱柱上等度洗脱分离,采用紫外检测器检测。结果标准曲线在0.1~2.0 mg/kg范围内线性良好。小麦基质中脱氧雪腐镰刀菌烯醇的回收率为72.8%~110.1%,精密度为3.6%~10.8%,实验室内Hor Rat值为0.24~0.48;玉米中脱氧雪腐镰刀菌烯醇的回收率为72.2%~90.6%,精密度为1.2%~5.2%,实验室内Hor Rat值为0.07~0.31。小麦基质中雪腐镰刀菌烯醇的回收率为58.9%~100.4%,精密度为3.6%~11.3%,实验室内Hor Rat值为0.23~0.63;玉米中雪腐镰刀菌烯醇的回收率为56.9%~91.9%,精密度为2.5%~7.8%,实验室内Hor Rat值为0.11~0.43。结论该方法具有灵敏度高、重现性好、操作简便、准确可靠等特点,适用于小麦和玉米中脱氧雪腐镰刀菌烯醇与雪腐镰刀菌烯醇的测定。
Objective To establish a method for the determination of deoxynivalenol and snow rot Fusarium enolase in wheat and maize by high performance liquid chromatography (HPLC). Methods The samples were extracted with pure water, purified with immunoaffinity column, eluted with methanol and eluted with isocratic elution on C18 column and detected by UV detector. Results The calibration curve was linear over the range of 0.1-2.0 mg / kg. The recoveries of deoxynivalenol in wheat matrix ranged from 72.8% to 110.1%, with a precision of 3.6% -10.8%. The laboratory Hor Rat values ranged from 0.24 to 0.48. The deoxynivalenol The recoveries ranged from 72.2% to 90.6% with a precision of 1.2% -5.2%. The laboratory Hor Rat values ranged from 0.07 to 0.31. The recovery rates of snow rot Fusarium enolase in wheat substrate ranged from 58.9% to 100.4%, the precision was 3.6% ~ 11.3%, and the Hor Rat in laboratory was 0.23 ~ 0.63. The recovery rate of Fusarium enolase in corn 56.9% ~ 91.9%, the precision was 2.5% ~ 7.8%, and the laboratory Hor Rat value was 0.11 ~ 0.43. Conclusion The method has the characteristics of high sensitivity, good reproducibility, simple operation, accuracy and reliability. It is suitable for the determination of deoxynivalenol and snow rot Fusarium enolase in wheat and corn.