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超高效液相色谱-串联质谱测定食品中4种真菌毒素残留量
引用本文:崔勇,李青,刘思洁,等. 超高效液相色谱-串联质谱测定食品中4种真菌毒素残留量[J]. 中国卫生工程学, 2014, 0(1): 46-48,51
作者姓名:崔勇  李青  刘思洁  
作者单位:吉林省卫生监测检验中心理化检验所,吉林长春130062
摘    要:目的建立同时检测食品中3-乙酰脱氧雪腐镰刀菌烯醇(3-ADON)、15-乙酰脱氧雪腐镰刀菌烯醇(15-ADON)、雪腐镰刀菌烯醇(NIV)和脱氧雪腐镰刀菌烯醇(DON)的超高效液相色谱一串联质谱(UPLC-MS/Ms)分析方法。方法采用WatersAcquityUPLCBEHC18色谱柱(1.7μm,50mm×2.1mm)、乙腈一0.1%氨水流动相、柱温35℃、质谱采用电喷雾电离(ESI)多反应监测(MRM)负离子模式进行检测,样品以乙腈一水为提取溶剂,经C-18固体萃取吸附剂除去基质干扰,取10μl注入UPLC-MS/MS。结果3-乙酰脱氧雪腐镰刀菌烯醇(3-ADON)、15-乙酰脱氧雪腐镰刀菌烯醇(15-ADON)、雪腐镰刀菌烯醇(NIV)和脱氧雪腐镰刀菌烯醇(DON)在5~200μg/L范围内呈良好的线性关系,加标回收率在85.9%~109.8%,所测定的相对标准偏差在2.34%~5.20%之间。结论该方法灵敏、快速,经济,结果准确可靠,可为食品中4种真菌毒素检测提供可靠的分析方法。

关 键 词:食品  真菌毒素  超高效液相色谱-串联质谱  多反应监测

Simultaneous determination of four mycotoxins residue in food by ultra performance liquid chromatography- mass/mass spectrometry
Affiliation:CUI Yong, LI Qing , LIU Si -jie , ZHANG Guan- ying( Physical and Chemical Laboratory, Jilin Provincial Center for Sanitation Inspection and Test, Changchun Jilin 130062, China)
Abstract:Objective To develop an ultra performance liquid chromatography - mass/mass spectrometry method for the simultaneous determination of 3 - ADON, 15 - ADON, NIV and DON in food. Methods Conditions : column, Acquity UP- LC BEH C 18 ( 1. 7 Ixm,50 mm × 2. 1 mm) ; mobile phase, acetonitrile - 0. 1% ammonia water; column temperature, 35 ℃ ; The detection was carried on a mass spectrometer coupled with ESI and MRM negative mode. The analytes in food were ex- tracted with water - acetonitrile. The extract was cleaned up using Cls solid phase extraction sorbent, injection volume was 10 μl. Results The linearity of 3 -ADON, 15 -ADON, NIV and DON was good in the range of 5 -200 μg/L The recov- ery of the method was 85.9% - 109. 8% and relative standard deviation was 2. 34% - 5.20%. Conclusion The method is accurate, quick and reliable.
Keywords:Food  Mycotoxin  UPLC - MS/MS  MRM
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