QuEChERS结合UPLC-Q/Orbitrap HRMS法测定小麦粉中9种真菌毒素

建立QuEChERS-高效液相色谱-四极杆/静电轨道离子阱高分辨质谱法同时测定小麦粉中9种真菌毒素的方法.样品经2.0％甲酸-乙腈提取,QuEChERS盐包脱水盐析后,用dSPE净化管净化,超高效液相色谱分离,在正离子模式下进行检测.在全扫描模式下测定目标化合物的一级精密质量数,与理论精密质量数相比,相对偏差不大于1....

Determination of Nine Mycotoxins in Wheat Flour by QuEChERS-Ultra-high Performance Liquid Chromatography-Quadrupole/Orbitrap High-Resolution Mass Spectrometry

A method was developed for the simultaneous determination of nine mycotoxins in wheat flour by ultra-high performance liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometry (UPLC-Q/Orbitrap HRMS) combined with QuEChERS (quick, easy, cheap, effective, rugged and safe) pretreatment. Samples were extracted with acetonitrile/formic acid solution (98.0:2.0, V/V), salted out with a QuEChERS salt pocket, and then purified with a dispersive solid phase extraction (dSPE) tube. The target compounds were separated by UPLC and detected in the positive ion mode. Measured accurate mass-to-charge ratios of the nine mycotoxins were obtained in the full scan mode with a relative deviation not more than 1.91 × 10-6 compared to the theoretical value, indicating accurate qualitative analysis of these compounds. A tandem mass spectral library for simultaneous screening and quantitation of the mycotoxins was built based on characteristic fragment ions. The linear ranges were 0.25–100 μg/L for all target analytes. The limit of quantification (LOQ) ranged from 0.30 to 3.00 μg/kg. Average recoveries at three spiked levels were in the range of 70.2%-112.0% with relative standard deviation (RSD) of 0.2%–4.5%. This method is useful for the high-throughput screening and confirmation of mycotoxins in wheat flour.