基于质谱特征碎裂片段的乳制品中真菌毒素非定向筛查方法研究

Non-directional Screening of Mycotoxins in Dairy Products Based on Mass Spectrometry Characteristic Fragments

该研究采用超高效液相色谱-四极杆-静电场轨道离子阱质谱的数据依赖型扫描,对38种典型真菌毒素标准物质化合物色谱信息、分子离子和二级碎裂片段进行采集,建立了真菌毒素标准数据库并完成了裂解途径解析与特征碎裂片段筛选;采用数据非依赖扫描,获取可追溯的样品质谱信息,构建了乳制品中真菌毒素的非定向筛查方法。该方法确定限(CCα)和检测容量(CCβ)分别为0.01~0.36μg/kg与0.03~0.57μg/kg,回收率为81.9%~111%,相对标准偏差(RSD)为1.1%~6.1%。将所建立的方法用于40个批次巴氏杀菌乳、超高温瞬时灭菌乳、含乳饮料及婴幼儿配方乳粉中真菌毒素的筛查,结果显示该方法快速、简便,可实现乳制品中真菌毒素准确定性和定量。

In this work,an ultra-high performance liquid chromatography-quadrupole-orbitrap mass spectrometry was developed for non-directional screening of mycotoxins in dairy products.Under the mass spectrometry data-dependent scanning mode,the molecular ion mass-to-charge ratios,secondary fragmented fragments mass-to-charge ratios and retention times of 38 typical mycotoxins reference materials were collected.A standard database for mycotoxins was established,and the analysis on fragmentation path was completed.The characteristic fragment fragments were combined with the standard database for mycotoxins in a mass-spectrum-independent scanning mode to finally achieve a non-directional screening of mycotoxins in dairy products.The detection limit(CCα) and the detection capacity(CCβ) of this method were in the ranges of 0.01-0.36 μg/kg and 0.03-0.57 μg/kg,respectively.and the recoveries ranged from 81.9% to 111% with relative standard deviations of 1.1%-6.1%.The established method was used to screen 40 batches of pasteurized milk,ultra-high temperature instant sterilized milk,milk-containing beverages and infant formula milk powder.Results showed that the method was simple and rapid,and could meet the requirements for accurate determination and quantitation of mycotoxins in dairy products.