超高效液相色谱-三重四极杆/复合线性离子阱串联质谱法快速检测食物中毒样品中的毒黄素  

Rapid determination of toxoflavin in food poisoning samples by ultra-high performance liquid chromatography-triple quadrupole/liner ion trap tandem mass spectrometry

作　　者：张伟[1] 冯光伟 赵东阳[1] 张榕杰[1] ZHANG Wei;FENG Guang-wei;ZHAO Dong-yang;ZHANG Rong-jie(Henan Provincial Center for Disease Control and Prevention,Zhengzhou,Henan 450016,China)

机构地区：[1]河南省疾病预防控制中心,河南郑州450016

出　　处：《中国卫生检验杂志》2021年第15期1811-1813,1817,共4页Chinese Journal of Health Laboratory Technology

基　　金：河南省重点研发与推广专项项目(192102310406)。

摘　　要：目的建立食物中毒样品中毒黄素的超高效液相色谱-三重四极杆/复合线性离子阱串联质谱快速确证方法。方法样品经酸性甲醇提取后,采用固相萃取净化、富集,溶剂吹干,0.5 ml 0.1%的甲酸水复溶,过0.22μm滤膜上机检测。采用ACQUITY HSS T3色谱柱分离,0.1%甲酸水-0.1%甲酸乙腈体系梯度洗脱,多反应监测(MRM)检测。结果毒黄素在0.05 ng/ml~5.0 ng/ml浓度内线性关系良好,相关系数为0.9999。平均加标回收率为82.0%~99.2%,相对标准偏差(RSD)为0.7%~2.9%,方法检出限为0.004μg/kg。结论该方法快捷灵敏,准确性高,确证性强,可以为临床诊断食物中毒提供一种快速检测毒黄素的最终确证方法。Objective To establish a rapid method for determining toxoflavin in food poisoning samples by ultra-high perform⁃ance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry.Methods The samples were extracted by formic-methanol,purified and concentrated by solid phase extraction column.Target compound was re-dissolved in 0.5 ml water-0.1%formic acid after evaporated by nitrogen,and then the sample was analyzed.Separated on an ACQUITY HSS T3 column using acetonitrile-0.1%formic acid and water-0.1%formic acid as mobile phase,toxoflavin was identified in multi⁃ple reaction monitoring mode(MRM).Results The method showed a good linearity when the concentration of toxoflavin was within 0.05 ng/ml-5.0 ng/ml and the correlation coefficient was 0.9999.The spike recovery was in the range of 82.0%-99.2%,the RSD was 0.7%-2.9%,and the detection limit was 0.004μg/kg.Conclusion The method is rapid,sensitive,accurate and highly confirmatory,which can provide a final confirmation method for rapid detection of toxoflavin in clinical diag⁃nosis of food poisoning.

关 键 词：食物中毒 毒黄素 液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]