CAJ | 학술논문

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。
목적：대원량중옥미적매희동면역친화층석정화고효액상색보측정방법진행개진화연구。방법양품분쇄후경체적분수위84%적을정용액초성제취,채용면역친화주정화, C18색보주진행분리,이을정-수-갑순(46：46：8)위류동상,최후용고효액상색보형광검측기대옥미적매희동진행측정,격발파장위274 nm,발사파장위440 nm。결과재우화실험조건하,측득옥미적매희동적선성상관계수위0.9998,상대표준편차위5.24%～7.96%,검출한위5μg/kg,가표회수솔위92.6%～108.0%。결론개진후적방법괄용우상용시수면역친화주정화원량중옥미적매희동。
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).ResultsUnder 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 5μg/kg and the spiked recoveries were between 92.6%~108.0%.ConclusionThe proposed method is suitable for fast, accurate and sensitive detection of zearalenone in grain with various immunoiffinity columns in market .