Quantitative Analysis Of Three Kinds Of Mycotoxins In Distillers Dried Grains With Soluble By Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

With the development of social material civilization,food safety problem,especially mycotoxin pollution,has attracted more and more attention from society and government.The three kinds of mycotoxin including Vomiting toxin(DON),aflatoxin(AFT),zearalenone(ZEN)mainly pollute cereal crops such as maize,wheat and barley.After eating these contaminated cereals by mistake,people and animals will have a wide range of toxic effects,seriously endangering the health of human and animal.For the large production enterprises with corn as raw material,the detection of mycotoxins in Distillers Dried Grains with Soluble(DDGS)has attracted more and more attention.In recent years,liquid chromatography-mass spectrometry(LC-MS)detection technology has developed rapidly.Compared with traditional methods in the determination of trace compounds,it has unparalleled advantages of high sensitivity,accuracy and accuracy.Because of high accuracy and low detection limit,Ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS)is often used to detect trace harmful substances in food.The contents of DON and its acetyl derivatives,ZEN and AFT in DDGS were determined by UHPLC-MS.Through a large number of experiments,the optimal pretreatment method and testing conditions are determined.Compared with the results of the authoritative departments,the method has the advantages of cost savings,accuracy and efficiency,and can be used in the routine inspection of the enterprise.Methods:The samples were extracted by acetonitrile aqueous solution,supernatant purified and centrifuged.Part of matrix was purified by clean-up column,the purification of ZEN required adding trace glacial acetic acid.After separation carried out on a C18 analytical column,DON and its acetyl derivatives,ZEN were determined by mass spectrometry under negative ions multi-reaction monitoring mode.AFT was determined under positive ions mode.Result:(1)The contents of DON,3-AcDON and 15-AcDON were detected by external standard method.The standard curve showed good linearity over the concentration range of 10-320?g/mL(R~2>0.99).The limited of quantitative detection was 0.05?g/L.The accuracy of the method was confirmed with an average recovery ranging between 78.2 and 90.5%with RSD of 2.8(n=6).(2)The content of ZEN was detected by external standard method.The standard curve showed good linearity over the concentration range of 10-160?g/mL(R~2>0.99).The limited of quantitative detection was 0.02?g/L.The accuracy of the method was confirmed with an average recovery ranging between 80.6 and 95.5%with RSD of2.8(n=6).(3)The content of AFT-B1was detected by external standard method.The standard curve showed good linearity over the concentration range of 2-100?g/mL(R~2>0.99).The limited of quantitative detection was 0.01?g/L.The accuracy of the method was confirmed with an average recovery ranging between 76.0 and 81.8%with RSD of2.5(n=6).