固相萃取柱净化-超高效液相色谱-串联质谱法快速测定液态乳中14种真菌毒素  

Determination of 14 Mycotoxins in Liquid Milk by Solid-Phase Extraction Coupled with Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：孙晓冬 郝杰 毛婷 邵瑞婷 姜洁 SUN Xiaodong;HAO Jie;MAO Ting;SHAO Ruiting;JIANG Jie(Beijing Municipal Center for Food Safety Monitoring and Risk Assessment,Beijing 100094,China)

机构地区：[1]北京市食品安全监控和风险评估中心,北京100094

出　　处：《食品科学》2018年第18期292-301,共10页Food Science

基　　金：国家重点研发计划"国家质量基础的共性技术研究与应用"专项(2016YFF0203802);北京市科技计划项目(Z161100000616007)

摘　　要：建立使用固相萃取柱净化液态乳中14种真菌毒素(黄曲霉毒素B_1、黄曲霉毒素B_2、黄曲霉毒素G_1、黄曲霉毒素G_2、黄曲霉毒素M_1、赭曲霉毒素A、橘霉素、T-2毒素、杂色曲霉素、伏马毒素B_1、伏马毒素B_2、玉米赤霉烯酮、脱氧雪腐镰刀菌烯醇、青霉酸)多残留的超高效液相色谱-串联质谱检测方法。样品经含0.1%甲酸-乙腈沉淀蛋白和提取,固相萃取柱Oasis PRi ME HLB净化后,以0.1%甲酸溶液与乙腈为流动相,经ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,梯度洗脱,采用电喷雾-正离子多反应监测模式,外标法定量。结果表明:14种真菌毒素的定量限(R_(SN)≥10)为0.5~5μg/kg,高、中、低3个添加水平时,平均回收率为67.7%~112.7%,相对标准偏差为0.43%~7.28%。该方法的检测速度快,净化效果较好,基质干扰较少,灵敏度高,结果准确、可靠,可用于液态乳中真菌毒素的检测分析。A rapid method was established for detecting 14 mycotoxins(aflatoxin B1,aflatoxin B2,aflatoxin G1,aflatoxin G2,aflatoxin M1,ochratoxin A,citrinin,T-2 toxin,sterigmatocystin,fumonisin B1,fumonisin B2,zearalenone,deoxynivalenol,and penicillic acid)in liquid milk by solid-phase extraction coupled with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Samples were defatted and extracted with 0.1%formic acid acetonitrile and the extract was cleaned up with Oasis PRiME HLB solid-phase extraction column.The analytes were separated on HSS T3 column(2.1 mm×100 mm,1.8μm)with a mobile phase composed of 0.1%formic acid and acetonitrile using gradient elution.Detection was carried out by tandem mass spectrometry using positive ionization in the multiple-reaction monitoring(MRM)mode.An external standard method was applied for quantification.Results showed that the limits of quantitation(LOQs)of 14 mycotoxins in matrices were between 0.5 and 5μg/kg.Average recoveries at 3 different spiked levels were 67.7%–112.7%with relative standard deviation(RSD)of 0.43%–7.28%.With the advantages of rapidity,high purification efficiency,low matrix interference and accurate and reliable results,the method is useful for the analysis of mycotoxins in liquid milk.

关 键 词：液态乳 固相萃取柱 超高效液相色谱-串联质谱 真菌毒素 快速 

分 类 号：TS207.3[轻工技术与工程—食品科学]