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.
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)
出处
《食品科学》
EI
CAS
CSCD
北大核心
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)
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
liquid milk
solid-phase extraction column
ultra-performance liquid chromatography-tandem mass spectrometry
mycotoxins
rapid detection
