粮食中玉米赤霉烯酮的电子捕获气相色谱分析
DETERMINATION OF ZEARALENONE IN FOODSTUFFS AND FEEDSTUFFS BY GC WITH ELECTRON-CAPTURE DETECTOR
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摘要: 本文建立了粮食中玉米赤霉烯酮的电子捕获气相色谱方法。粮食样品经氯仿-醋酸乙酯(1:1)提取后浓缩,浓缩液用NaOH提取,NaOH提取液经HCI调至pH为3.5左右,过Sep-pak C18柱。用乙腈洗脱柱上玉米赤霉烯酮,洗脱液浓缩至干,残渣用七氟丁酸酐衍生化后进行气相色谱分析。结果表明,玉米赤霉烯酮在电子捕获气相色谱上的最低检出限为4×10-11g,相关系数为0.9996。在玉米、小麦、大麦、大米中的回收率在50ng/g—100ng/g的范围内均在80%以上。各粮食中的最低检出限均低于20ng/g。Abstract: A method to detect zearalenone in corn, wheat, rice and barley by gas-liquid chromatography with electron-capture detector was developed. Toxin was extracted with chloroform-ethyl acetate (1:1) and dissolved in aqueous NaOH solution. The solution was acidified to pH 3.5, passed through a Sep-pak C18 column,and eluted with acetonitrile. Zearalenone was detected quantitatively by GC after derivatized with heptafluorobutyric acid anhydride. Recovery of zearalenone from cereals was all above 80% at 50ng-100ng/g. The detection limit was less than 20ng/g.
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