超高效液相色谱-四极杆/静电场轨道阱高分辨质谱对粮谷产品中20种真菌毒素的快速筛查和确证

建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查和确证粮谷产品中20种真菌毒素的方法。样品经乙腈（含2%（体积分数）甲酸）提取，用Captiva EMR-Lipid小柱净化，采用Thermo Hypersil Gold C₁₈柱（100 mm×2.1 mm，1.9 μm）分离，用四极杆/静电场轨道阱高分辨质谱进行分析。在全扫描模式下以分析物的保留时间和一级母离子信息实现快速筛查，以自动触发采集的二级碎片离子信息进行确证。结果显示，目标分析物在各自的质量浓度范围内线性关系良好（相关系数r²>0.99），方法检出限为0.25~20 μg/kg，回收率为72.9%~117.8%，相对标准偏差为2.9%~15.2%（n=6）。该方法灵敏度高，结果准确、可靠，适用于粮谷产品中20种真菌毒素的快速筛查和确证。

Rapid screening and confirmation of 20 mycotoxins in grain products by ultrahigh performance liquid chromatography- quadrupole/electrostatic field orbitrap high- resolution mass spectrometry

A rapid method based on ultrahigh-performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry (UPLC-HRMS) was developed for the screening and confirmation of 20 mycotoxins in grain products. The samples were extracted with acetonitrile containing 2% (v/v) formic acid, and the extracts were cleaned up on Captive EMR-Lipid columns. The analytes were separated on a Thermo Hypersil Gold C₁₈ column (100 mm×2.1 mm, 1.9 μm), and analyzed by UPLC-HRMS. The retention time and accurate mass of the parent ion were used for fast screening in full scan mode, while the accurate masses of the fragment ions were used for confirmation in the two-stage threshold-triggered full mass scan mode. The results revealed that the 20 mycotoxins showed good linear relationships in their respective mass concentration ranges. The correlation coefficients were not less than 0.99, and the limits of quantitation (LOQs) ranged from 0.25 to 20 μg/kg. The recoveries of the 20 mycotoxins in the sample ranged from 72.9% to 117.8% with the relative standard deviations (RSDs) from 2.9% to 15.2% at three spiked levels (n=6). This method has the advantages of high sensitivity and reliability, and is thus suitable for the rapid screening and confirmation of 20 mycotoxins in grain products.