QuEChERS结合UPLC-MS/MS同时测定植物固体饮料中13种真菌毒素

Simultaneous Determination of 13 Mycotoxins in Plant Solid Beverages by UPLC-MS/MS Combined with Modified QuEChERS

本研究建立了一种基于QuEChERS前处理结合超高效液相色谱串联质谱(UPLC-MS/MS)定量分析的高通量检测方法,用于测定植物固体饮料中的13种真菌毒素。样品均质加水溶解后,采用QuEChERS法进行前处理,以2%甲酸-乙腈溶液超声提取,十八烷基硅烷键合硅胶(C18)进行除杂净化。提取液经Kinetex F5色谱柱分离后,采用串联质谱多反应监测模式(MRM)进行检测,基质匹配标准曲线法进行定量。结果显示,13种真菌毒素在测试范围内均呈现良好的线性关系(r>0.9916),检出限在0.04~16.9μg/kg之间,定量限在0.12~38.2μg/kg之间,精密度(RSD)小于9.0%,且在植物固体饮料中的加标回收率在82.2%到103.3%之间。利用该方法对18份植物固体饮料样品进行筛查,其中检出4份样品含有真菌毒素,包括脱氧雪腐镰刀菌烯醇和伏马毒素B3。该方法具有操作简便、成本低、灵敏度高和准确度高的优势,可满足植物固体饮料中多种真菌毒素的高通量筛查。

This work aimed to develop a high-throughput analytical method based on QuEChERS coupled with ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)for the determination of 13 mycotoxins in plant-solid beverages.The samples were homogenized and dissolved in water.QuEChERS method was used for pretreatment,ultrasonic extraction with 2%formic acid-acetonitrile solution,and purification with octadecylsilane bonded silica gel(C18).The extraction solution was then separated by a Kinetex F5 column,detected by a tandem mass spectrometry detector in multiple reaction monitoring mode(MRM),and quantified by matrix-matched standard calibration.The optimum conditions achieved limits of detections(LODs)in the range of 0.04~16.9μg/kg,with correlation coefficient over 0.9916.The limit of quantifications(LOQs)were in the range 0.12~38.2μg/kg.The recoveries in real plant-solid beverages ranged from 82.2%to 103.3%,with relative standard deviations(RSDs)below 9.0%.Moreover,the proposed method was applied to analyze mycotoxins in 18 plant-solid beverage samples,a positive detection rate of 4/18 was obtained,and the detected analytes included deoxynivalenol and fumonisin B3.This proposed method has the advantages of simple operation,low cost,high sensitivity and accuracy,which can be used for the high-throughput screening of multiple mycotoxins in plant-solid beverages.