高分辨质谱法对坚果类食品中55种真菌毒素的快速筛查和确证

Rapid screening and identification of 55 mycotoxins in nut foods by high resolution mass spectrometry

旨在建立QuEChERS-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坚果类食品中55种真菌毒素的方法。试样用1%乙酸乙腈提取,改进的QuEChERS法净化,经Accucore RP-MS色谱柱分离,通过高分辨质谱一级全扫描(Full-MS)和二级扫描(dd-MS^(2))进行定性、定量分析。检测的55种真菌毒素方法检出限为0.05~7.5μg/kg,定量限为0.1~15μg/kg;在最低点与最高点相差20倍浓度范围内有良好的线性关系,r^(2)≥0.990;55种真菌毒素在不同基质和不同浓度水平的加标回收率为70.3%~120.0%,相对标准偏差为0.3%~18.4%(n=6)。本方法灵敏度高、重现性和稳定性良好,可满足坚果类食品中多种真菌毒素的高通量快速筛查和定量检测。

The method of QuEChERS ultra high performance liquid chromatography quadrupole/electrostatic field orbital trap high resolution mass spectrometry was established.The samples were extracted with 1%acetic acid in acetonitrile solution,purified by improved QuEChERS method.The mycotoxins were separated by Accucore RP-MS liquid chromatography column,qualitatively and quantitatively analyzed by Full-MS and dd-MS^(2) mode.The detection limit of 55 mycotoxins was 0.05-7.5μg/kg,with a quantification limit of 0.1-15μg/kg.There was a good linear relationship within the range of 20 times the difference between the lowest point and the highest point,r^(2)≥0.990.The recovery rates of 55 mycotoxins in different substrates and concentrations were 70.3%-120.0%,with a relative standard deviations of 0.3%-18.4%(n=6).This method has high sensitivity,good reproducibility and stability,and can meet the high throughput rapid screening and quantitative detection of many mycotoxins in nut foods.