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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 C_(18)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~(-11)g,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。
In this paper, an electron capture GC method for determining zearalenone in grain has been established. Food samples were extracted with chloroform-ethyl acetate (1: 1) and concentrated. The concentrate was extracted with NaOH. The NaOH extract was adjusted to pH 3.5 by HCI and passed through a Sep-Pak C 18 column. The zearalenone was eluted from the column with acetonitrile. The eluate was concentrated to dryness. The residue was derivatized with heptafluorobutyric anhydride and analyzed by gas chromatography. The results showed that the minimum detectable limit of detection of zearalenone by gas chromatography was 4 × 10 ~ (-11) g with a correlation coefficient of 0.9996. The recoveries in corn, wheat, barley, and rice are over 80% in the range of 50 ng / g to 100 ng / g. The minimum detection limit of each grain is less than 20ng / g.