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通过液相色谱-串联质谱法(LC-MS/MS)比较稳定同位素稀释分析法(SIDA)与基质匹配校准法对四种食品基质中霉菌毒素的定量分析

Quantitation of Mycotoxins in Four Food Matrices Comparing Stable Isotope Dilution Assay (SIDA) with Matrix-Matched Calibration Methods by LC-MS/MS.

作者信息

Li Dan, Steimling Justin A, Konschnik Joseph D, Grossman Scott L, Kahler Ty W

机构信息

Restek Corp., 110 Benner Circle, Bellefonte, PA 16823.

出版信息

J AOAC Int. 2019 Nov 1;102(6):1673-1680. doi: 10.5740/jaoacint.19-0028. Epub 2019 Apr 2.

DOI:10.5740/jaoacint.19-0028
PMID:30940286
Abstract

Mycotoxins are big concerns in food safety. Analytical methods are important for the evaluation of mycotoxins in different food commodities. In this study, stable isotope dilution assay (SIDA) was compared with a matrix-matched calibration method for the quantification of mycotoxins in four different commercially available commodities and two reference materials. All samples were extracted with water-acetonitrile (50+50, v/v), followed by filtration and LC-tandem MS analysis. SIDA calibration accuracies ranged from 78.6 to 112% with relative SDs (RSDs) ≤16% across all four matrices. The majority of the recoveries across all matrices ranged from 70 to 120% with RSDs <11%. Of the four mycotoxins in the reference materials analyzed, only three had C-internal standard (IS), whereas the fourth was quantified using a closely eluting C-IS for a different mycotoxin. Mycotoxins paired with their corresponding C-IS had accuracies >90%, whereas accuracies for the mismatched mycotoxin/C-IS were <14%. When C-IS are not available, matrix-matched calibration was also evaluated as an alternative to quantitating target mycotoxins. The use of C-IS is the best way to dynamically account for prevalent matrix effects, but matrix matching provides a viable alternative. The study compared SIDA and matrix-matched calibration methods in terms of recovery, efficiency, advantages, and limitations for LC-MS based mycotoxin analysis.

摘要

霉菌毒素是食品安全中的重大问题。分析方法对于评估不同食品中的霉菌毒素很重要。在本研究中,将稳定同位素稀释分析法(SIDA)与基质匹配校准法进行了比较,以对四种不同的市售商品和两种参考物质中的霉菌毒素进行定量分析。所有样品均用水 - 乙腈(50 + 50,v/v)萃取,然后过滤并进行液相色谱 - 串联质谱分析。在所有四种基质中,SIDA校准准确度范围为78.6%至112%,相对标准偏差(RSDs)≤16%。所有基质中的大多数回收率范围为70%至120%,RSDs <11%。在分析的参考物质中的四种霉菌毒素中,只有三种有碳内标(IS),而第四种则使用与另一种霉菌毒素紧密洗脱的碳内标进行定量。与相应碳内标配对的霉菌毒素准确度>90%,而不匹配的霉菌毒素/碳内标组合的准确度<14%。当没有碳内标时,也评估了基质匹配校准作为定量目标霉菌毒素的替代方法。使用碳内标是动态考虑普遍存在的基质效应的最佳方法,但基质匹配提供了一种可行的替代方法。该研究在回收率、效率、优点和局限性方面比较了SIDA和基质匹配校准法用于基于液相色谱 - 质谱的霉菌毒素分析。

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