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目的对原粮中玉米赤霉烯酮免疫亲和层析净化高效液相色谱测定方法进行改进和研究。方法样品粉碎后经体积分数为84%的乙腈溶液超声提取,采用免疫亲和柱净化,C18色谱柱进行分离,以乙腈-水-甲醇(46:46:8)为流动相,最后用高效液相色谱荧光检测器对玉米赤霉烯酮进行测定,激发波长为274 nm,发射波长为440 nm。结果在优化实验条件下,测得玉米赤霉烯酮的线性相关系数为0.9998,相对标准偏差为5.24%~7.96%,检出限为5μg/kg,加标回收率为92.6%~108.0%。结论改进后的方法适用于常用市售免疫亲和柱净化原粮中玉米赤霉烯酮。
Objective To improve and study the determination of zearalenone in raw milk by immunoaffinity chromatography. Methods After the sample was crushed, the sample was extracted by acetonitrile with a volume fraction of 84%, and purified by immunoaffinity column. The residue was separated on a C18 column with mobile phase of acetonitrile - water - methanol (46: 46: 8) The chromatographic fluorescence detector was used to determine zearalenone at an excitation wavelength of 274 nm and an emission wavelength of 440 nm. Results Under the optimized experimental conditions, the linear correlation coefficient of zearalenone was 0.9998, the relative standard deviation was 5.24% ~ 7.96%, the detection limit was 5μg / kg and the recoveries were 92.6% -108.0%. Conclusion The improved method is suitable for the purification of zearalenone in raw grains by commonly used commercial immunoaffinity column.