QuEChERS/LC-MS/MS法测定食品中7种真菌毒素 |
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基金项目:国家质检总局科技计划项目(2016IK050) |
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中文摘要:建立了食品中常见的黄曲霉毒素B1(AFB1)、黄曲霉毒素B2(AFB2)、黄曲霉毒素G1(AFG1)、黄曲霉毒素G2(AFG2)、赭曲霉毒素A(OTA)、赭曲霉毒素B(OTB)和赭曲霉毒素C(OTC)7种真菌毒素的QuEChERS前处理净化结合液相色谱-串联质谱(LC-MS/MS)检测方法。样品用甲酸-乙腈(10∶90)进行酸化稀释,离心后取上清液经吸附净化剂(1.2 g MgSO4+0.25 g C18+0.4 g PSA+0.25 g Al-N)富集净化,过滤后采用LC-MS/MS在多反应监测(MRM)模式下测定。7种真菌毒素在各自范围内线性良好,相关系数(r)均不小于0.999。在最佳条件下,方法的定量下限(LOQ)为0.25~5.0 μg/kg,7种毒素的相对标准偏差(RSD,n=6)为1.1%~7.7%,平均回收率为71.5%~119%。该方法操作方便、灵敏度高、重现性好,能满足大批量食品中上述7种真菌毒素残留的检测要求。 |
中文关键词:QuEChERS 真菌毒素 赭曲霉毒素 黄曲霉毒素 高效液相色谱-串联质谱(LC-MS/MS) |
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Detection of Seven Mycotoxins in Foods by LC-MS/MS with QuEChERS |
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Abstract:A method of liquid chromatograph-tandem mass spectrometry(LC-MS/MS) with QuEChERS pretreatment was developed for the determination of seven kinds of mycotoxins,including aflatoxin B1(AFB1),aflatoxin B2(AFB2),aflatoxin G1(AFG1),aflatoxin G2(AFG2),ochratoxin A(OTA),ochratoxin B(OTB) and ochratoxin C(OTC) in foods.The samples were diluted with formic acid-acetonitrile (10∶90,by volume),and then purified by QuEChERS using a scavenging agent(1.2 g MgSO4+0.25 g C18+0.4 g PSA+0.25 g Al-N) after centrifugation.The detection on the analytes was performed by LC-MS/MS in positive ionization under multiple-reaction monitoring(MRM) mode.There existed good linearities for seven mycotoxins in their respective concentraction ranges with correlation coeffieionts not less than 0.999.The limits of quantitation(LOQs) were in the range of 0.25-5.0 μg/kg,and the average recoveries for seven mycotoxins were between 71.5% and 119% with the relative standard deviations(RSDs,n=6) of 1.1%-7.7%.The developed method was simple,sensitive and reproducible,and was suitable for the determination of these mycotoxins in foods in batch production. |
Key Words:QuEChERS mycotoxin ochratoxins aflatoxins LC-MS/MS |
引用本文:熊欣,刘青,张广文,庞世琦,曾广丰,陈文锐.QuEChERS/LC-MS/MS法测定食品中7种真菌毒素[J].分析测试学报,2018,37(9):1008-1013. |
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