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目的建立饼干中4种单端孢霉烯类真菌毒素的液相色谱-质谱联用分析方法。方法样品经乙腈/水溶液(84:1 6,V:V)提取后用MycoSep227或MycoSep226多功能柱净化,Agilent ZORBAX Bonus-RP色谱柱分离,液相色谱-质谱联用(LC-MS/MS)测定,电喷雾正离子模式(ESI~+)和负离子模式(ESI~-)多反应模式检测。结果样品中4种单端孢霉烯类真菌毒素在各自的线性范围内线性关系良好,相关系数均不低于0.997,定量限为5~20μg/kg,3个加标水平下平均回收率为66.9%~1 01.8%,相对标准偏差为3.7%~13.9%。结论该方法具有前处理简单、净化效果好、灵敏度高,适用于同时检测一种样品中4种单端孢霉烯类真菌毒素的残留量。
Objective To establish a liquid chromatography-mass spectrometry method for the analysis of four trichothecene mycotoxins in biscuits. Methods The samples were extracted with acetonitrile / water (84: 1, V: V) and purified with MycoSep227 or MycoSep226 multifunctional column, separated on an Agilent ZORBAX Bonus-RP column and analyzed by liquid chromatography-mass spectrometry (LC- MS / MS), electrospray positive ion mode (ESI ~ +) and negative ion mode (ESI ~ -). Results The linearity of the four trichothecene mycotoxins in the samples was good. The correlation coefficient was no less than 0.997 and the limit of quantification was 5 ~ 20μg / kg. The average recoveries of the three trichothecenes were 66.9% ~ 1 01.8%, the relative standard deviation was 3.7% ~ 13.9%. Conclusion The method has the advantages of simple pretreatment, good purification effect and high sensitivity, and is suitable for simultaneous detection of four kinds of trichothecene mycotoxin residues in one sample.