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

中文关键词:  超高效液相色谱-串联质谱  玉米油  玉米赤酶烯酮

英文关键词:ultra performance liquid chromatography-mass spectrometry  corn oil  zearalenon

中文摘要:

      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 ACQUITY BEH (2.1 mm×100 mm,1.7 μm)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2~100 μg/L浓度范围内呈良好的线性关系, 在5、20、80 μg/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1.0 μg/kg, 定量限为3.0 μg/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。

英文摘要:

      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 (2.1 mm×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.