| 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 |
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| 基金项目:国家自然科学基金资助项目(31801643)；陕西省科技计划项目(2019NY-117,2020NY-097)；西安市未央区科技计划项目(201936)；2019年国家级大学生创新创业训练计划资助项目(201910708007) |
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| 中文摘要: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0.01~0.36 μg/kg与0.03~0.57 μg/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。 |
| 中文关键词:乳制品 真菌毒素 超高效液相色谱-四极杆-静电场轨道离子阱质谱 非定向筛查 |
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| Non-directional Screening of Mycotoxins in Dairy Products Based on Mass Spectrometry Characteristic Fragments |
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| Abstract: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. |
| Key Words:dairy products mycotoxin ultra high performance liquid chromatography-quadrupole-orbitrap mass spectrometry non directional screening |
| 引用本文：贾玮，樊子便，杜安，石琳，许牡丹，储晓刚.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[J].分析测试学报,2020,39(6):705-714. |
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