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利用轨道阱质谱法同时测定小麦粉中的总麦角生物碱。

Simultaneous determination of total ergot alkaloids in wheat flour by Orbitrap mass spectrometry.

机构信息

Food Analysis Research Center, Korea Food Research Institute, Republic of Korea.

Food Analysis Research Center, Korea Food Research Institute, Republic of Korea.

出版信息

Food Chem. 2024 May 30;441:138363. doi: 10.1016/j.foodchem.2024.138363. Epub 2024 Jan 7.

DOI:10.1016/j.foodchem.2024.138363
PMID:38199100
Abstract

The optimization screening methods for total ergot alkaloids in wheat extracts involve transforming them into a single compound, which is then analyzed via high-resolution Orbitrap mass spectrometry (Orbitrap MS). Orbitrap MS provides highly sensitive and accurate mass measurements, enhancing the selectivity and sensitivity of the analysis. Various hydrolysis and reduction methods have been investigated, and the use of superhydrides has emerged as the most effective method for transforming ergopeptine alkaloids. This study also focused on the epimerization of ergot alkaloids, particularly the differences between R- and S-epimers and their impact on the mass spectra. We validated our method by assessing the linearity, sensitivity, recovery, matrix effects, repeatability, and stability. The limits of detection and quantitation were set at 0.43 and 1.30 μg LSA/kg wheat, respectively. The proposed method offers a robust analytical approach for screening and quantifying total ergot alkaloids in wheat samples, addressing important concerns about their presence in food and feed.

摘要

小麦提取物中单种麦角生物碱的优化筛选方法涉及将其转化为单一化合物,然后通过高分辨轨道阱质谱(Orbitrap MS)进行分析。Orbitrap MS 提供了高灵敏度和准确的质量测量,提高了分析的选择性和灵敏度。已经研究了各种水解和还原方法,超氢化物的使用已成为转化麦角生物碱最有效的方法。本研究还集中在麦角生物碱的差向异构化上,特别是 R-和 S-差向异构体的差异及其对质谱的影响。我们通过评估线性度、灵敏度、回收率、基质效应、重复性和稳定性来验证我们的方法。检测限和定量限分别设定为 0.43 和 1.30μg LSA/kg 小麦。该方法为筛选和定量小麦样品中的总麦角生物碱提供了一种稳健的分析方法,解决了食品和饲料中存在这些物质的重要问题。

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