高效液相色谱法定量检测玉米油中玉米赤霉烯酮的溶剂萃取预处理方法研究

Solvent extraction pretreatment for determination of zearalenone in maize oil by HPLC

研究了高效液相色谱法(HPLC)定量检测精炼玉米油中玉米赤霉烯酮(ZEN)的溶剂萃取预处理方法,优化了溶剂萃取预处理条件并进行了方法的评估。结果表明:溶剂萃取预处理的最优条件为乙腈-水(体积比9∶1)混合溶液萃取、料液比1∶4、超声萃取时间20 min,该萃取预处理条件可实现ZEN准确定量测定,检出限达4.5μg/kg;10、100、1 000μg/m L加标水平下的加标回收率分别为77.9%、105.7%、95.0%,相对标准偏差2.05%~8.43%,优于传统免疫亲和柱净化预处理方法。

The solvent extraction pretreatment method for determination of zearalenone （ZEN） in refined maize oil by HPLC （ SE - HPLC） was established and assessed. The resuhs showed that the optimal con- ditions of solvent extraction pretreatment were obtained as follows ： with 90% acetonitrile water solution as extraction solution, ratio of material to liquid 1：4 and ultrasonic extraction time 20 min. The extraction pretreatment conditions realized the accurately quantitative determination of ZEN. The detection limit of SE - HPLC method was 4.5 μg/kg. The mean recoveries of the target compounds （ spiked at three con- centration levels ： 10, 100 μg/kg and 1 000 μg/kg） were 77.9%, 105.7% and 95.0% respectively and the relative standard deviations （RSDs） were ranged from 2.05% to 8.43%. Through comparative anal- ysis, the method was better than traditional immune affinity column pretreatment method.