多功能针式过滤器净化超高效液相色谱法测定大米和花生中玉米赤霉烯酮

Determination of zearalenone in rice and peanuts by ultra high performance liquid chromatography with multifunctional needle filter purification

建立了一种基于多功能针式过滤器净化的超高效液相色谱测定大米和花生中玉米赤霉烯酮的方法。样品经乙腈提取,采用多功能针式过滤器通过式净化,以超高效液相色谱法测定其中的玉米赤霉烯酮,色谱柱为ACQUITY UPLC BEH C_(18)柱(100 mm×2.1 mm,1.7μm),以甲醇-乙腈-水(体积比为8∶46∶46)为流动相等度洗脱,流量为0.3 mL/min,用荧光检测器检测,色谱峰面积外标法定量。玉米赤霉烯酮的质量浓度在2.5~500 ng/mL范围内与色谱峰面积线性关系良好,相关系数不小于0.9995。大米和花生样品的方法检出限分别为15.0、30.0μg/kg,定量限分别为50.0、100.0μg/kg。样品加标回收率为77.11%~93.65%,测定结果的相对标准偏差为0.49%~4.95%(n=6)。该方法简便快速,适用于大米和花生中玉米赤霉烯酮的日常检测。

A method for the determination of zearalenone in rice and peanuts by ultra high performance liquid chromatography based on multifunctional needle filter purification was established.The sample was extracted with acetonitrile and purified through a multifunctional needle filter.The content of zearalenone in the sample was determined by ultra high performance liquid chromatography.The chromatographic column was ACQUITY UPLC BEH C_(18)column(100 mm×2.1 mm,1.7μm),methanol-acetonitrile-water(volume ratio 8∶46∶46)was used as the mobile phase with isocratic elution,the flow rate was 0.3 mL/min.Extraction solution was detected by a fluorescence detector,and quantified by the chromatographic peak area external standard method.The mass concentration of zearalenone had a good linear relationship with the chromatographic peak area in the range of 2.5-500 ng/mL,and the correlation coefficient was not less than 0.9995.The detection limits for rice and peanut samples were 15.0μg/kg,and 30.0μg/kg,respectively,and the quantification limits were 50.0μg/kg and 100.0μg/kg,respectively.The recoveries of sample spiking were 77.11%-93.65%,and the relative standard deviations of the determination results were 0.49%-4.95%(n=6).The method has the advantages of simple and fast,which is suitable for the daily detection of zearalenone in rice and peanut.