同位素稀释-超高效液相色谱串联质谱法快速测定植物油中16种真菌毒素  

Rapid determination of 16 mycotoxins in vegetable oil by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：张宇 李俊玲[1] 王书舟[1] 张伟[2] ZHANG Yu;LI Jun-ling;WANG Shu-zhou;ZHANG Wei(Anyang Municipal Center for Disease Control and Prevention,Anyang,Henan 455000,China;不详)

机构地区：[1]河南省安阳市疾病预防控制中心,河南安阳455000 [2]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16期1921-1926,共6页Chinese Journal of Health Laboratory Technology

基　　金：河南省2019科技发展计划项目(192102310406);安阳市2018科技发展计划科技攻关项目(2018-78)。

摘　　要：目的建立植物油中16种真菌毒素的同位素稀释超高效液相色谱-串联质谱快速检测方法。方法样品中加入乙腈-水-甲酸(79∶20∶1,V/V/V)溶液提取,10000 r/min离心5 min后直接稀释,再经高速低温离心后加入同位素内标,C18柱(2.1 mm×100 mm,1.8μm)分离,通过四级杆串联质谱仪电喷雾离子化和MRM多重反应离子监测模式检测,内标法定量。结果16种真菌毒素在其各自的线性范围内具有良好的线性关系,相关系数r均>0.996,方法检出限为0.10μg/kg~10μg/kg,定量限为0.30μg/kg~30μg/kg,高、中、低3个浓度的加标回收率在88.3%~104.6%,RSD在1.1%~7.4%。对市售植物油40份进行测定,结果显示AFB1、ZEN和FB1阳性检出率较高,分别为40%、20%和17.5%。结论该方法具有良好的精密度和准确度,前处理方法简单、省时,可以满足植物油中16种真菌毒素快速检测的日常工作需求。Objective To establish a method for the rapid determination of 16 mycotoxins in vegetable oil by isotope dilution ultra-high performance liquid chromatography-tandem mass spectrometry. Methods The sample was extracted by adding acetonitrile-water-formic acid( 79∶20∶1,V/V/V) solution,centrifuged for 5 min at 10 000 r/min,then directly diluted,then centrifuged at high speed and low temperature,and separated on a C18 column( 2. 1 mm × 100 mm,1. 8 μm). The samples were detected by electrospray ionization with four-stage series mass spectrometer and multiple reactive ion monitoring by MRM,and quantified by internal standard method. Results The 16 mycotoxins had a good linear relationship within the linear range,and the correlation coefficients were all greater than 0. 996. The detection limits of the method were within0. 10 μg/kg-10 μg/kg,and the quantitative limits were within 0. 30 μg/kg-30 μg/kg. The recoveries of the three spiked levels were within 88. 3%-104. 6%,and the RSDs were within 1. 1%-7. 4%,respectively. 40 samples of vegetable oils sold in the market were tested,and the results showed that the positive rates of AFB1,ZEN and FB1 were 40%,20% and 17. 5%,respectively. Conclusion The method has good precision and accuracy,and the pretreatment method is simple and time-saving,and can meet the daily needs of rapid detection of 16 mycotoxins in vegetable oil.

关 键 词：植物油 真菌毒素 同位素稀释 超高效液相色谱-串联质谱法 

分 类 号：O657[理学—分析化学]