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中国精品科技期刊2020
陆智,李亚贤,刘凤松,等. QuEChERS结合UPLC-MS/MS同时测定植物固体饮料中13种真菌毒素[J]. 华体会体育,2024,45(21):275−282. doi: 10.13386/j.issn1002-0306.2023120099.
引用本文: 陆智,李亚贤,刘凤松,等. QuEChERS结合UPLC-MS/MS同时测定植物固体饮料中13种真菌毒素[J]. 华体会体育,2024,45(21):275−282. doi: 10.13386/j.issn1002-0306.2023120099.
LU Zhi, LI Yaxian, LIU Fengsong, et al. Simultaneous Determination of 13 Mycotoxins in Plant Solid Beverages by UPLC-MS/MS Combined with Modified QuEChERS[J]. Science and Technology of Food Industry, 2024, 45(21): 275−282. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023120099.
Citation: LU Zhi, LI Yaxian, LIU Fengsong, et al. Simultaneous Determination of 13 Mycotoxins in Plant Solid Beverages by UPLC-MS/MS Combined with Modified QuEChERS[J]. Science and Technology of Food Industry, 2024, 45(21): 275−282. (in Chinese with English abstract). 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

  • 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.

     

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