高效液相色谱法测定原粮中玉米赤霉烯酮的

Improvement research on determination of zearalenonein grain by high per-formance liquid chromatography

中文关键词:  高效液相色谱法  免疫亲和柱  玉米赤霉烯酮  原粮

英文关键词:high performance liquid chromatography  immunoaffitnity column  zearalenone  grain

中文摘要:

      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。

英文摘要:

      Objective To improve immunoaffinity column clean-up and high performance liquid chromatography (HPLC) method for the determination of zearalenone in grain. Methods Ground sample was extracted with 84% acetonitrile solution (v:v) by ultrasonic wave. The chromatographic purification was performed on an immunoaffinity column and separated on a C18 column, using a mixture of acetonitrile, water and ethanol (v:v:v=46:46:8) as mobile phase, then the analyte was detected by HPLC with fluoresence detector (Ex=274 nm, Em=440 nm). Results Under the optimal conditions, the correlation coefficient (r) was more than 0.9998. The relative standard deviations (RSDs) were in the range of 5.24%~7.96%, the limit of detection (LOD) was 5 μg/kg and the spiked recoveries were between 92.6%~108.0%. Conclusion The proposed method is suitable for fast, accurate and sensitive detection of zearalenone in grain with various immunoiffinity columns in market .