分析化学2016，Vol.44Issue(11)：1728-1734,7.DOI:10.11895/j.issn.0253-3820.160408
同位素稀释-超高效液相色谱-线性离子阱串联质谱分析谷物及其制品中呕吐毒素及其衍生物和代谢物
Analysis of Deoxynivalenol and Related Derivatives and Metabolites in Cereal and Cereal Products by Ultra Performance Liquid Chromatography-Quadrupole Linear Ion Trap Mass Spectrometry with Isotopic Dilution
摘要
Abstract
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® 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 1-300μg/L. The limits of detection (LOD) and quantitation (LOQ) were 0. 1 μg/kg and 0. 3 μg/kg, respectively. The mean recovery was 81. 3%-101. 7% at three spiked levels of 5, 50, 200μg/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.关键词
同位素稀释/呕吐毒素及其衍生物和代谢物/超高效液相色谱/线性离子阱串联质谱Key words
Isotopic dilution/Deoxynivalenol and its derivatives and metabolites/Ultra performance liquid chromatography/Quadrupole linear ion trap mass spectrometry引用本文复制引用
刘柱,华颖,徐潇颖,陈万勤,赵超群,梁晶晶,丁宇琦,罗金文..同位素稀释-超高效液相色谱-线性离子阱串联质谱分析谷物及其制品中呕吐毒素及其衍生物和代谢物[J].分析化学,2016,44(11):1728-1734,7.基金项目
本文系浙江省科技计划项目(No.2015C37054)、浙江省科技厅重大科技专项重大农业项目(No.2014C02001)、浙江中医药大学校级科研基金项目(No.2015ZR10)资助 （No.2015C37054）
