Mycotoxin Research ( IF 2.6 ) Pub Date : 2022-04-08 , DOI: 10.1007/s12550-022-00455-1 Sophie Scheibenzuber 1 , Fabian Dick 1 , Marina Bretträger 2 , Martina Gastl 2 , Stefan Asam 1 , Michael Rychlik 1
A liquid chromatography tandem mass spectrometry (LC–MS/MS) multi-mycotoxin method was developed for the analysis of the Alternaria toxins alternariol (AOH), alternariol monomethyl ether (AME), tentoxin (TEN), altertoxin I (ATX I), altertoxin II (ATX II), alterperylenol (ALTP), and altenuene (ALT), as well as the modified toxins AOH-3-glucoside (AOH-3-G), AOH-9-glucoside (AOH-9-G), AME-3-glucoside (AME-3-G), AOH-3-sulfate (AOH-3-S), and AME-3-sulfate (AME-3-S) in barley and malt. The toxin tenuazonic acid (TeA) was analyzed separately as it could not be included into the multi-mycotoxin method. Quantitation was conducted by using a combination of stable isotope dilution analysis (SIDA) for AOH, AME, and TeA, and matrix-matched calibration for all other toxins. Limits of detection were between 0.05 µg/kg (AME) and 2.45 µg/kg (ALT), whereas limits of quantitation ranged from 0.16 µg/kg (AME) to 8.75 µg/kg (ALT). Recoveries between 96 and 107% were obtained for the analytes when SIDA was applied, while recoveries between 84 and 112% were found for analytes quantified by matrix-matched calibration. The method was applied for the analysis of 50 barley samples and their respective malts from the harvest years 2016–2020 for their mycotoxin content, showing the overall potential of toxin formation during the malting process. The toxins ALTP and ATX I were mainly found in the malt samples, but not in barley.
中文翻译:
开发分析方法以研究麦芽制作对大麦中游离和修饰形式的链格孢霉菌毒素水平的影响
开发了一种液相色谱串联质谱 (LC-MS/MS) 多霉菌毒素方法来分析链格孢属毒素 交替萜醇 (AOH)、交替萜醇单甲醚 (AME)、tentoxin (TEN)、交替毒素 I (ATX I)、交替毒素 II (ATX II)、交替萜酚 (ALTP) 和交替烯 (ALT),以及修饰的毒素 AOH -3-葡萄糖苷 (AOH-3-G)、AOH-9-葡萄糖苷 (AOH-9-G)、AME-3-葡萄糖苷 (AME-3-G)、AOH-3-硫酸盐 (AOH-3-S) ,以及大麦和麦芽中的 AME-3-硫酸盐 (AME-3-S)。毒素tenuazonic acid (TeA) 单独分析,因为它不能包含在多霉菌毒素方法中。通过对 AOH、AME 和 TeA 使用稳定同位素稀释分析 (SIDA) 和对所有其他毒素的基质匹配校准相结合来进行定量。检测限在 0.05 µg/kg (AME) 和 2.45 µg/kg (ALT) 之间,而定量限从 0.16 µg/kg (AME) 到 8.75 µg/kg (ALT)。当应用 SIDA 时,分析物的回收率在 96% 到 107% 之间,而通过基质匹配校准量化的分析物的回收率在 84% 到 112% 之间。该方法用于分析 2016-2020 年收获年的 50 个大麦样品及其各自麦芽的霉菌毒素含量,显示了麦芽制造过程中毒素形成的总体潜力。毒素 ALTP 和 ATX I 主要存在于麦芽样品中,但未在大麦中发现。