超高效液相色谱-串联质谱法测定食品中脱氧雪腐镰刀菌烯醇的方法优化

Optimization of determination of deoxynivalenol in foods by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  脱氧雪腐镰刀菌烯醇  质控样  超高效液相色谱-串联质谱法

英文关键词:deoxynivalenol  quality control sample  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 优化超高效液相色谱-串联质谱法测定食品中脱氧雪腐镰刀菌烯醇含量的分析方法。方法 样品经粉碎匀质后, 采用70%乙腈-甲酸水溶液涡旋浸泡提取, 普瑞邦亲和柱净化, 以乙腈-0.05%氨水作为流动相, Waters BEH C18柱(2.1 mm×100 mm, 1.7 μm)进行色谱分离, 超高效液相色谱-串联质谱的多反应监测(multiple reaction monitoring, MRM)模式进行测定, 内标法定量。结果 脱氧雪腐镰刀菌烯醇在5.0~150.0 μg/L范围内具有良好的线性关系(r2=0.9995), 添加回收率为93.4%~101.6%, 相对标准偏差为1.41%~3.54%, 质控样检测值在参考值允许范围内(569±60) μg/kg, 具有较好的重现性和准确度。结论 本研究提升了脱氧雪腐镰刀菌烯醇的检测能力, 该方法准确、可靠、便捷, 可满足实验要求。

英文摘要:

      Objective To optimize the method for determination of deoxynivalenol in foods by ultra performance liquid chromatography-tandem mass spectrometry. Methods After crushing and homogenizing, the sample was extracted with 70% acetonitrile formic acid aqueous solution by vortex immersion and purified by PriboLab affinity column. The mobile phase was acetonitrile-0.05% ammonia. Waters BEH C18 (2.1 mm×100 mm, 1.7 μm) was used for chromatography separation. Then it was determined by ultra performance liquid chromatography-tandem mass spectrometry with multiple reaction monitoring mode and quantitative analyzed by internal standard method. Results Deoxynivalenol had a good linear relationship (r2=0.9995) in the concentration range of 5.0~150.0 μg/L. Addition recovery rate was 93.4%–101.6%, and relative standard deviation was 1.41%–3.54%. The control sample detection value has a good reproducibility and accuracy within the allowable range of reference values (569±60) μg/kg. Conclusion This study can improve the detection ability of deoxynivalenol. This method is accurate, reliable and convenient, and can meet the requirements of experiment.