Albert Julius, More Camilla A, Dahlke Niklaus R P, Steinmetz Zacharias, Schaumann Gabriele E, Muñoz Katherine
iES Landau, Institute for Environmental Sciences, Group of Organic and Ecological Chemistry, University of Koblenz-Landau, Fortstraße 7, 76829 Landau, Germany.
iES Landau, Institute for Environmental Sciences, Group of Environmental and Soil Chemistry, University of Koblenz-Landau, Fortstraße 7, 76829 Landau, Germany.
ACS Omega. 2021 Jul 16;6(29):18684-18693. doi: 10.1021/acsomega.1c01451. eCollection 2021 Jul 27.
Aflatoxins (AFs) are toxic fungal secondary metabolites that are commonly detected in food commodities. Currently, there is a lack of generic methods capable of determining AFs both at postharvest stages in agricultural products and preharvest stages, namely, the agricultural soil. Here, we present a simple and reliable method for quantitative analysis of AFs in soil and food matrices at environmentally relevant concentrations for the first time, using the same extraction procedure and chromatography, either by HPLC-FLD or LC-MS. AFs were extracted from matrices by ultrasonication using an acetonitrile/water mixture (84:16, v + v) without extensive and time-consuming cleanup procedures. Food extracts were defatted with -hexane. Matrix effects in terms of signal suppression/enhancement (SSE) for HPLC-FLD were within ±20% for all matrices tested. For LC-MS, the SSE values were mostly within ±20% for soil matrices but outside ±20% for all food matrices. The sensitivity of the method allowed quantitative analysis even at trace levels with quantification limits (LOQs) between 0.04 and 0.23 μg kg for HPLC-FLD and 0.06-0.23 μg kg for LC-MS. The recoveries ranged from 64 to 92, 74 to 101, and 78 to 103% for fortification levels of 0.5, 5, and 20 μg kg, respectively, with repeatability values of 2-18%. The validation results are in accordance with the quality criteria and limits for mycotoxins set by the European Commission, thus confirming a satisfactory performance of the analytical method. Although reliable analysis is possible with both instruments, the HPLC-FLD method may be more suitable for routine analysis because it does not require consideration of the matrix.
黄曲霉毒素（AFs）是有毒的真菌次生代谢产物，在食品中普遍被检测到。目前，缺乏能够同时测定农产品收获后阶段和收获前阶段（即农业土壤）中AFs的通用方法。在此，我们首次提出了一种简单可靠的方法，用于定量分析土壤和食品基质中环境相关浓度的AFs，使用相同的提取程序和色谱法，可通过高效液相色谱-荧光检测器（HPLC-FLD）或液相色谱-质谱联用（LC-MS）。AFs通过超声处理从基质中提取，使用乙腈/水混合物（84:16，v + v），无需繁琐且耗时的净化程序。食品提取物用正己烷脱脂。对于HPLC-FLD，所有测试基质的信号抑制/增强（SSE）方面的基质效应在±20%以内。对于LC-MS，土壤基质的SSE值大多在±20%以内，但所有食品基质的SSE值超出±20%。该方法的灵敏度使得即使在痕量水平也能进行定量分析，HPLC-FLD的定量限（LOQs）在0.04至0.23 μg/kg之间，LC-MS的定量限在0.06 - 0.23 μg/kg之间。对于0.5、5和20 μg/kg的加标水平，回收率分别为64%至92%、74%至101%和78%至103%，重复性值为2%至18%。验证结果符合欧盟委员会设定的霉菌毒素质量标准和限量，从而证实了该分析方法的令人满意的性能。虽然使用这两种仪器都可以进行可靠的分析，但HPLC-FLD方法可能更适合常规分析，因为它不需要考虑基质。
