QuEChERS-超高效液相色谱-串联质谱法测定玉米糁中呕吐毒素  

Determination of deoxynivalenol in corn grits by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：李敏 贺姗姗 王宏宇 LI Min;HE Shan-shan;WANG Hong-yu(College of Food and Bioengineering,Zhengzhou University of Light Industry,Zhengzhou 450001,Henan,China;Key Laboratory of Cold Chain Food Processing and Safety Control,Ministry of Education,Zhengzhou University of Light Industry,Zhengzhou 450001,Henan,China)

机构地区：[1]郑州轻工业大学食品与生物工程学院,河南郑州450001 [2]郑州轻工业大学冷链食品加工与安全控制教育部重点实验室,河南郑州450001

出　　处：《粮食与油脂》2025年第3期149-154,共6页Cereals & Oils

基　　金：河南省科技攻关项目(242102111066)。

摘　　要：建立一种以MIL-101(Fe)为吸附剂的QuEChERS前处理法结合超高效液相色谱-串联质谱法(UPLC-MS/MS)测定玉米糁中呕吐毒素(DON)的方法。以乙腈-水(体积比80∶20,含体积分数1%乙酸)为提取溶剂,提取方式为涡旋1 min+离心(8000 r/min)3 min;采用60 mg MIL-101(Fe)以涡旋3 min+离心(8000 r/min)3 min方式净化。结果表明:呕吐毒素在质量浓度为10~1000 ng/mL范围内线性关系良好,回收率为80.3%~87.1%,日内相对标准偏差为2.0%~4.5%,日间相对标准偏差为6.3%,检出限为0.50 ng/mL,定量限为0.67 ng/mL。建立的方法快速省时、操作简便、灵敏度高、重现性好,适用于玉米糁中呕吐毒素的测定。A QuEChERS pretreatment method using MIL-101(Fe)as adsorbent combined with ultrahigh performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)for the determination of deoxynivalenol(DON)in corn grits was established.Acetonitrile-water(volume ratio 80∶20,containing 1%acetic acid by volume)was used as the extraction solvent,and the extraction method was vortex for 1 minand centrifugation(8000 r/min)for 3 min.Purification was carried out using 60 mg MIL-101(Fe)by vortex for 3 min and centrifugation(8000 r/min)for 3 min.The results showed that the linear relationship of DON was good within the mass concentration range of 10-1000 ng/mL,with a recovery rate of 80.3%-87.1%,intra day relative standard deviation of 2.0%-4.5%,inter day relative standard deviation of 6.3%,detection limit of 0.50 ng/mL,and quantification limit of 0.67 ng/mL.The established method was fast,time-saving,easy to operate,highly sensitive,and reproducible,suitable for the determination of DON in corn grits.

关 键 词：MIL-101(Fe) QUECHERS 超高效液相色谱-串联质谱 玉米糁 呕吐毒素 

分 类 号：TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程]