高效液相色谱同步检测小麦中脱氧雪腐镰刀菌烯醇和玉米赤霉烯酮的方法研究

Simultaneous Determination of Deoxynivalenol and Zearalenone in Wheat by High Performance Liquid Chromatography

文章建立了二合一免疫亲和柱净化、紫外检测器串联荧光检测器的高效液相色谱同步检测小麦中脱氧雪腐镰刀菌烯醇和玉米赤霉烯酮的方法。样品用60%乙腈水提取,涡旋、振荡、离心、过滤等步骤,滤液过二合一免疫亲和柱净化,甲醇洗脱后氮气吹干,50%甲醇水复溶上机分析。该方法可在25 min内完成2种真菌毒素的同步检测,脱氧雪腐镰刀菌烯醇和玉米赤霉烯酮的线性关系r值均大于0.999。在不同水平的加标试验中,脱氧雪腐镰刀菌烯醇和玉米赤霉烯酮的回收率分别是85.8%~95.5%和87.8%~92.3%,相对标准偏差分别是3.2%~7.8%和3.2%~7.5%,检出限分别是50μg/kg和5μg/kg,定量限分别是100μg/kg和10μg/kg。该方法用外标法进行定量检测,灵敏度高、操作简单,准确性和重复性好。

The method for simultaneous determination of deoxynivalenol(Don) and zearalenone(Zen) in wheat using a two in one immunoaffinity column purification and high performance liquid chromatography with UV detector and fluorescence detector in series was established.The samples were extracted with 60% acetonitrile water,followed by vortexing,shaking,centrifugation,filteration,and the filtrate was purified using a two in one immunoaffinity column.The solution dried by N2 and redissolved by 50% methanol water was detected by a high performance liquid chromatography coupled with a fluorescence detector and an ultraviolet detector.This method can complete the simultaneous detection of two mycotoxins within 25 minutes,and the average correlation of calibration curves for Don and Zen exceeding 0.999.The average recovery rates were 85.8%–95.5% and 87.8%–92.3%%,the relative standard deviations(RSD) were 3.2%–7.8% and 3.2%–7.5%,and the limits of detection were 50 μg/kg and 5 μg/kg,the limits of quantification were 100 μg/kg and 10 μg/kg.This method was sensitive,rapid and exact by the external standard method.