液相-电喷雾质谱法测定饲料中脱氧雪腐镰刀菌烯醇的残留量

Determination of Dexynivalenol in feed by liquid chromatography coupled with electrospray ionization tandem mass spectrometry

建立了液相-电喷雾串联质谱法检测饲料中的脱氧血腐镰刀菌烯醇（DON）。样品用磷酸盐缓冲液（pH7．0）提取，经cts固相萃取净化、5％甲醇再溶解后进行LC-MS／MS分析。质谱采用电喷雾离子源，正离子多重反应监测模式进行定量和定性分析。色谱柱采用PhenomenexLuna5μC18（2），流动相为甲醇-O．1％甲酸溶液（30：70）。方法的检测限为20μg，kg，定量限为50μg／kg；在50、250、500μg／kg等3个浓度水平．回收率为75．4％-93．2％，相对标准偏差为5．74％-7．62％。

A method has been developed for the determination of Dexynivalenol in feed by liquid chromatography coupled with eleetrospray ionization tandem mass spectrometry. The samples were extracted by phosphate buffer （pH 7.0） and purified by C18 solid phase extraction, and then analyzed by the LC-MS/MS after redissolved by 5% methanol. The mass spectrometry was run with electrospray ion source and in positive ions multiple reaction monitoring mode for the quantitative and qualitative analysis. The chromatographic column was a Phenomenex Luna 5μC18（2）, and the flowing phase was comprised with methanol- 0.1% formic acid solution （30：70）. Limit of detection （LOD） was 20μg/kg, and the limit of quantitation （LOQ） was 50μg/kg. The recoveries ranged from 75,4% to 93.2% in 50, 250 and 500μg/kg concentration level. The relative standard deviation ranged from 5.74% to 7.62%.