液相色谱-四极杆/静电场轨道阱高分辨质谱测定植物油中8种真菌毒素

Determination of 8 Mycotoxins in Plant Oil by Quadrupole Tandem Orbitrap High-resolution Mass Spectrometry

本研究建立了高效液相色谱-静电场轨道阱选择离子扫描质谱快速测定植物油中黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、黄曲霉毒素M1、赭曲霉毒素A、伏马毒素B2、玉米赤霉烯酮8种真菌毒素的方法。样品采用氯化钠盐析,甲醇-水(70∶30,v/v)溶液提取,正己烷除脂,经振荡、超声、离心和过滤前处理后即可进行测定,无需进一步净化。采用电喷雾正离子选择离子全扫描模式,基质外标法定量测定8种真菌毒素。在优化的实验条件下,8种真菌毒素浓度与对应峰面积线性关系良好,相关系数r≥0.9975,定量限在0.2~5.0μg/kg之间,方法回收率为72.4%~108.3%,相对标准偏差(n=6)在3.5%~15.0%之间。结果表明,该方法操作简单、灵敏度高,能够满足植物油中多种真菌毒素的快速检测要求。

A method employing liquid chromatography-quadruplole tandem orbitrap high resolution mass spectrometry(Q-Exactive Targeted MS/MS) was developed to simultaneously analyze aflatoxins B1,B2,G1,G2,M1,ochratoxin A,fumonisin B2,zearalenone in plant oil.The plant oil sample underwent salting out with sodium chloride,followed by extraction with methanol-water(70:30,v/v) and defatting with n-hexane.After oscillation,ultrasound,centrifugation and filtration,samples can be measured without further purification.The analytes were determined by mass spectrometry using electrospray ionization in positive select ion full scanning mode and the quantification was implemented with matrix external standard method.The proposed method demonstrated excellent linear correlation with the correlation coefficients all above 0.9975.The limits of quantification(LOQs) ranged from 0.2 μg/kg to 5.0 μg/kg.The recovery rates ranged from 72.4% to 108.3%,with relative standard deviations(RSDs) between 3.5% and 15.0%.The method offers advantages in both simplicity and sensitivity,making it suitable for the rapid determination of mycotoxins in plant oil.