免疫亲和柱-高效液相色谱法测定谷物及其制品中玉米赤霉烯酮的含量

Determination of zearalenone in corn and its products by immunoaffinity column-high performance liquid chromatography

目的建立免疫亲和柱-高效液相色谱法分析检测谷物及其制品中玉米赤霉烯酮的方法。方法样品经乙腈-去离子水(84:16,V:V)提取,玉米赤霉烯酮免疫亲和柱富集净化,甲醇洗脱后,经C18反相色谱柱分离,以乙腈-水-甲醇(46:46:8,V:V:V)为流动相,使用高效液相色谱-荧光检测器检测,外标法定量。结果玉米赤霉烯酮在1~100μg/L线性范围内线性关系良好,相关系数0.9999,检出限0.8μg/kg,仪器重复测定的相对标准偏差0.19%,样品平行性测定相对标准偏差在0.10%~1.89%。检测成都市内综合农贸市场和超市内谷物及其制品中玉米赤霉烯酮的含量为1.34~43.1μg/kg,检出率为52.2%。结论该方法具有灵敏度高、重现性好、准确度高等特点,可应用于实际市场中谷物及其制品的痕量调查。

Objective To establish a method for determination of zearalenone in corn and its products by immunoaffinity-high performance liquid chromatography.Method The samples were extracted with acetonitrile-deionized water(84:16,V:V),enriched and purified by zearalenone immunoaffinity column.After eluting with methanol,they were separated by C18 reversed-phase chromatography column using acetonitrile-water-methanol(46:46:8,V:V:V)as the mobile phase,detected by high performance liquid chromatography-fluorescence detector,and quantified by external standard method.Results Zearalenone had a good linear relationship in the linear range of 1–100μg/L,with a correlation coefficient of 0.9999,and limit of detection was 0.8μg/kg.The relative standard deviation of the instrument repeated determination was 0.19%,and the relative standard deviation of the sample parallelism determination were 0.10%–1.89%.The contents of zearalenone in cereals and their products in comprehensive farmers’markets and supermarkets in Chengdu were 1.34–43.1μg/kg,and the detection rate was 52.2%.Conclusion This method had the advantages of high sensibility,good repeatability and high accuracy.It was fit for the trace analysis in the grain and its products in actual market investigation.