超快速液相色谱-串联质谱法测定粮食及食用油中的黄曲霉毒素

摘要

The artiole applied a rapid method for determinationof aflatoxins B1,B2,G1and G2 in grain and edibleoil by ultra fast liquidchromatography tandem mass spectrometry(UFLC–MS/MS) and provided analytical methodology for the flour,corn andoil in Ningxia province. Samplesof flour,corn andoil were ultrasonically extracted by acetonitrile–water(20︰80) solution,cleaned up by immunity affinitycolumn. The aflatoxins B1,B2,G1and G2 were separatedon Atlantis T3chromatographic column with mobile phaseof methanol –0.1% formic acidon gradientelution. The aflatoxins B1,B2,G1 and G2 qualified and quantified by mass spectrometry. The analysisof aflatoxins B1,B2,G1and G2 were could be detected in 6 minutes by UFLC–MS/MS,and the average recoveriesof them in wheat,corn andoil samples at three spiked levels were 75.6%~94.1% with relative standard deviations less than 10.0%. The limitof detection(LOD) and the limitof quantitation(LOQ) for the whole method were 0.05μg/kg and 0.15μg/kg. The method was accurate,reliable,andcould be used as a qualitycontrol method for aflatoxins B1,B2,G1and G2 in grain and edibleoil.%应用超快速液相色谱―串联质谱法技术，建立粮食及食用油中黄曲霉毒素的检测方法，并对宁夏市售小麦粉、玉米制品和食用油进行分析。样品经乙腈―水（20︰80）提取，免疫亲和柱净化；以甲醇–0.1%甲酸水溶液为流动相，用Atlantis T3色谱柱分离，以电喷雾正离子模式进行质谱测定。采用该方法，黄曲霉毒素B1、B2、G1和G2可在6分钟内完成检测，分别以小麦粉、玉米制品和食用油为加标基质，三个加标水平下的平均回收率为75.6%~94.1%，相对标准偏差小于10.0%，检出限（S/N=3）为0.05μg/kg，定量限（S/N=10）为0.15μg/kg。该方法操作快速简单、重现性好，可用于粮食中黄曲霉毒素B1、B2、G1和G2的检测。