超高效液相色谱-串联质谱法测定玉米油中玉米赤酶烯酮的残留量

Determination of zearalenon residue in corn oil by ultra performance liquid chromatography-mass/mass spectrometry

目的建立玉米油中玉米赤酶烯酮检测的超高效液相色谱-串联质谱（UPLC-MS/MS）分析方法。方法样品经乙腈超声提取,经免疫亲和柱进行净化,采用Waters ACQITY BEH（2.1 mm×100 mm,1.7μm）色谱柱分离,以0.1%氨水溶液和乙腈为流动相进行梯度洗脱;质谱以负离子模式扫描和多反应监测（MRM）模式进行检测,以内标法定量。结果玉米赤酶烯酮在2~100μg/L浓度范围内呈良好的线性关系,在5、20、80μg/kg 3个添加水平下,加标回收率为90.2%~105.1%,相对标准偏差为1.66%~3.50%。玉米赤霉烯酮的检出限为1.0μg/kg,定量限为3.0μg/kg。结论本方法灵敏、结果准确可靠,可适用于玉米油中玉米赤酶烯酮的检测。

Objective To establish a method for determination of zearalenon in corn oil by ultra performance liquid chromatography-mass/mass spectrometry（UPLC-MS/MS）.Methods The samples were extracted by ultrasonic with acetonitrile,purified with immune affinity column,separated by Waters ACQUITY BEH column（2.1mm×100 mm,1.7 μm） with the gradient elution using the mobile phase of acetonitrile and 0.1%ammonia.Negative ion mode scanning and multiple reactions monitoring（MRM） were used in MS,and internal standard method was used for quantification.Results Zearalenon had a good linear relationship in the range of 2~100 μg/L.The recoveries were ranged from 90.2%to 105.1%for the zearalenon residues with 3 spiked levels of 5,20,80 μg/kg,and the relative standard deviations（RSD） were 1.66%~3.50%.The detection limit was 1.0 μg/kg,and the limit of quantification was 3.0 μg/kg.Conclusion The method is accurate,sensitive and reliable,which is suitable for the determination of zearalenon residue in corn oil.