高效液相法同时检测谷物中玉米赤霉烯酮和赭曲霉毒素A

Simultaneous Determination of Ochratoxin A and Zearalenone in Cereals by HPLC

该研究开发一种快速、灵敏同时检测玉米、小麦和稻米中玉米赤霉烯酮(zearalenone,ZEN)和赭曲霉毒素A(ochratoxin A,OTA)的高效液相色谱检测方法。将样品采用乙腈/水(80/20,体积比),200 r/min,30℃振荡提取30 min后,经Oasis PRiME HLB固相萃取柱净化后,上样检测。该方法ZEN和OTA检测限(limit of detection,LOD)为3.7μg/kg和0.11μg/kg,定量限(quantification Limit,LOQ)为12.25μg/kg和0.38μg/kg,线性范围分别为10μg/kg^2000μg/kg和0.2μg/kg^200μg/kg,加标样品中不同浓度的ZEN和OTA回收率为83.0%~101.3%,日内精密度和日间精密度分别为3.12%~7.03%和3.57%~9.3%。该方法适用于玉米、小麦和稻米中ZEN和OTA的同时检测。

A sensitive and rapid method had been developed for the simultaneous determination of ochratoxin A(OTA)and zearalenone(ZEN)in corn,wheat and rice by high performance liquid chromatography(HPLC).After extraction with acetonitrile and water(80/20,volume ratio)for 30 min under 30°C and 200 r/min in a rotary shaker,the cereal samples were purified using Oasis PRiME HLB cartridge.The limits of detection and quantification of the mycotoxins were determined under the optimum HPLC conditions at 3.7μg/kg and12.25μg/kg for ZEN and 0.11μg/kg and 0.38μg/kg for OTA,respectively.High correlation coefficients(R2>0.99)were obtained in the range of 10μg/kg-2000μg/kg for ZEN and 0.2μg/kg-200μg/kg for OTA.The average recoveries ranged from 83.0%to 101.3%for different concentrations of ZEN and OTA in spiked samples along with good intra-day(3.12%-7.03%)and inter-day(3.57%-9.3%)precision.The method proposed is suitable for the simultaneous determination of ZEN and OTA and can be performed for the mycotoxin analysis in corn,wheat and rice.