食品工业科技2024,Vol.45Issue(21) :275-282.DOI:10.13386/j.issn1002-0306.2023120099

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

陆智 李亚贤 刘凤松 高智 李亚杰
食品工业科技2024,Vol.45Issue(21) :275-282.DOI:10.13386/j.issn1002-0306.2023120099

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

陆智 1李亚贤 1刘凤松 1高智 1李亚杰1
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作者信息

  • 1. 无限极(中国)有限公司,广东 广州 510405
  • 折叠

摘要

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0.04~16.9 μg/kg之间,定量限在0.12~38.2 μg/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.

Abstract

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 0.04~16.9 μg/kg,with correlation coefficient over 0.9916.The limit of quantifications(LOQs)were in the range 0.12~38.2 μg/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.

关键词

QuEChERS/超高效液相色谱串联质谱法/真菌毒素/植物固体饮料/高通量

Key words

QuEChERS/ultra-performance liquid chromatography-tandem mass spectrometry/mycotoxins/plant solid beverages/high-throughput

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出版年

2024
食品工业科技
北京一轻研究院

食品工业科技

CSTPCD北大核心
影响因子:0.842
ISSN:1002-0306
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