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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 the determination of corn laminarinase in corn oil by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods The samples were extracted by acetonitrile and purified by immunoaffinity column. The samples were separated on a Waters ACQUITY BEH (2.1 mm × 100 mm, 1.7 μm) column and eluted with 0.1% aqueous ammonia solution and acetonitrile as mobile phase. Negative ion mode scanning and multiple reaction monitoring (MRM) mode were performed and quantified by internal standard method. Results Corn alkenone showed a good linearity in the concentration range of 2 ~ 100 μg / L. The spiked recoveries were 90.2% ~ 105.1% at 5, 20, and 80 μg / kg levels with relative standard deviations 1.66% ~ 3.50%. The detection limit of zearalenone was 1.0μg / kg and the limit of quantification was 3.0μg / kg. Conclusion The method is sensitive, the results are accurate and reliable, and can be applied to the detection of maize erythroketene in corn oil.