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摘要
A method was established for the qualitative identification and quantitative determination of DON, 3-Ac-DON, 15-Ac-DON, DOM-1 in cereal and cereal products based on solid phase extraction and ultra performance liquid chromatography-quadrupole linear ion trap mass spectrometry (UPLC-QTRAP-MS/MS) with isotopic dilution. Samples were extracted by the mixture of acetonitrile and water (84 : 16, V/V), degreased by hexane saturated with acetonitrile and purified by HLB solid phase extraction cartridge. The target analytes were separated by Waters Atlantis (R) T3 column with gradient elution by mobile phases which consisted of acetonitrile and 0. 02% ammonia water. A scheduled multiple reaction monitoring (MRM) in negative mode as survey scan and an enhanced product ion (EPI) scan as dependent scan in an information dependent acquisition (IDA) experiment were adopted in mass spectrometry acquisition. On. line lab. built MS/MS library as well as the isotope internal standards was employed for the identification and qualification. For each analyte, the correlation coefficient was above 0. 999 in the linear range of 1-300 mu g/L. The limits of detection (LOD) and quantitation (LOQ) were 0. 1 mu g/kg and 0. 3 mu g/kg, respectively. The mean recovery was 81. 3% -101. 7% at three spiked levels of 5, 50, 200 mu g/kg. The relative standard deviation (RSD) was no more than 5%. The proposed method was successfully applied to the analysis of FAPAS's QC samples and five representative samples. This method was simple, fast and precise, and suitable for the determination and confirmation of deoxynivalenol and its derivatives and metabolites in cereal and cereal products.
- 出版日期2016-11
- 单位浙江中医药大学
