液相色谱-串联质谱法同时测定动物血浆中21种霉菌毒素或其代谢物残留

建立了同时检测动物血浆中黄曲霉毒素B1等21种霉菌毒素或其代谢物残留的液相色谱-串联质谱方法.动物血浆样品中加入0.1％甲酸-乙腈溶液、NaCl和无水MgSO4进行萃取,无水MgSO4和C18,PSA,A-AL对提取液进行脱水净化,经浓缩、复溶和离心后,再进行测定.采用反相C18色谱柱分离,以0.1％甲酸-0.5 mmol/L乙酸铵溶液和0.1％甲酸-甲醇溶液作为流动相进行梯度洗脱,采用电喷雾离子源(ESI)多反应监测离子模式(MRM)进行检测,基质标准曲线外标法进行定量分析,线性范围在0.05 ～ 100 ng/mL之间,方法的定量限为0.05 ～0.5 ng/mL.在高、中、低3个添加浓度水平下,21种霉菌毒素的平均回收率为62.0％ ～ 116.4％,相对标准偏差小于19％.

Simultaneous Detection of 21 Kinds of Mycotoxins and Their Metabolites in Animal Plasma with Impurity Adsorption Purification Followed by Liquid Chromatography-Tandem Mass Spectrometry

A novel method for simultaneous detection of mycotoxins (e.g.,aflatoxin B1) or their metabolic residues in animal plasma with impurity adsorption purification followed ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed.Extraction of mycotoxins and their metabolites from animal plasma sample was performed with 0.1％ formic acid-acetonitrile solution after addition of sodium chloride and hydrous magnesium sulfate.The extract was then dehydrated and purified with hydrous magnesium sulfate,C18,primary secondary amine,and alumina-A.3 mL of the supernatant was evaporated and re-dissolved with 0.5 mL of 0.1％ formic acid aqueous solution/acetonitrile (70∶ 30,V/V) for UPLC-MS/MS detection.The analytes were separated by a C18 column utilizing gradient elution with 0.1％ formic acid aqueous solution containing 0.5 mmol of ammonium acetate and 0.1％ formic acid-methanol solution,and finally detected by tandem mass spectrometry in positive/negative ESI mode.Identification and quantification were achieved by LC-MS/MS with multi-reaction monitoring (MRM).Good linearity in response was obtained in the analytes concentration range of 0.05-100 ng/mL with correlation coefficients larger than 0.99.The limits of quantification (S/N=10) were around 0.05-0.5 ng/mL.The recoveries of mycotoxins and their metabolites spiked in blank plasma samples were in the range of 62.0％-116.4％,with relative standard deviations (RSDs) less than 19.0％.