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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

Simultaneous determination of four mycotoxins residue in food by ultra performance liquid chromatography- mass /mass spectrometry

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【作者】 崔勇李青刘思洁张冠英

【Author】 CUI Yong;LI Qing;LIU Si-jie;ZHANG Guan-ying;Physical and Chemical Laboratory,Jilin Provincial Center for Sanitation Inspection and Test;

【机构】 吉林省卫生监测检验中心理化检验所

【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-串联质谱(UPLC-MS/MS)分析方法。方法采用Waters Acquity UPLC BEH C18色谱柱(1.7μm,50 mm×2.1 mm)、乙腈-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-水为提取溶剂,经C18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。

【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 UPLC BEH C 18( 1. 7 μm,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 extracted with water- acetonitrile. The extract was cleaned up using C 18 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 recovery 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.

【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
【Key words】 FoodMycotoxinUPLC-MS /MSMRM
  • 【文献出处】 中国卫生工程学 ,Chinese Journal of Public Health Engineering , 编辑部邮箱 ,2014年01期
  • 【分类号】O657.63;TS207.4
  • 【被引频次】5
  • 【下载频次】172
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