Division of Organic Trace and Food Analysis, Department of Analytical Chemistry, Reference Materials, Bundesanstalt für Materialforschung und -prüfung (BAM), Richard-Willstätter-Str. 11, D-12489 Berlin, Germany.
Toxins (Basel). 2022 Aug 11;14(8):549. doi: 10.3390/toxins14080549.
Rapid, cost-efficient, and eco-friendly methods are desired today for routine analysis of the mycotoxin zearalenone (ZEN) in edible vegetable oils. Liquid chromatography with fluorescence detection (HPLC-FLD) is commonly used to reliably control the specified ZEN maximum levels, which requires efficient sample clean-up to avoid matrix interferences. Therefore, a highly selective extraction and clean-up method based on reversible covalent hydrazine chemistry (RCHC) using hydrazine-functionalized silica was developed. This efficient solid-phase extraction (SPE) involves reversible hydrazone formation of ZEN with the hydrazine moiety covalently bound to a solid phase. Optimal conditions were achieved with 1 mL SPE cartridges filled with 400 mg of hydrazine-functionalized silica. The developed RCHC-SPE method was validated in an interlaboratory comparison study (ILC) with twelve participants analyzing six edible vegetable oils with a focus on maize oils. The derived method parameters (ZEN recovery 83%, repeatability 7.0%, and reproducibility 18%) meet the performance criteria of Commission Regulation (EC) No 401/2006. The developed RCHC-SPE-based HPLC-FLD method allows the reliable quantification of ZEN in the range of 47-494 µg/kg for different types of edible vegetable oils, also for matrix-reach native oils. Due to the high efficiency, the significantly reduced matrix load helps to extend the lifetime of analytical equipment. Furthermore, the re-useability of the RCHC-SPE cartridges contributes to an eco-friendly approach and reduced analysis costs. To our knowledge, this is the first report on ZEN quantification in edible vegetable oils based on manual RCHC-SPE cartridges. Due to its high performance, the developed RCHC-SPE method is a promising alternative to the current European standard method EN 16924:2017 (HPLC-FLD part).
今天,人们希望开发快速、经济高效且环保的方法,以常规分析食用植物油中的真菌毒素玉米赤霉烯酮(ZEN)。液相色谱法与荧光检测(HPLC-FLD)通常用于可靠地控制规定的 ZEN 最大水平,这需要有效的样品净化以避免基质干扰。因此,开发了一种基于可逆共价腙化学(RCHC)的高度选择性萃取和净化方法,该方法使用肼功能化硅胶。这种高效的固相萃取(SPE)涉及 ZEN 与肼部分通过可逆腙形成与固相共价结合。在填充有 400mg 肼功能化硅胶的 1ml SPE 小柱中,可达到最佳条件。在一项有 12 个参与者的实验室间比较研究(ILC)中,对六种食用植物油(重点是玉米油)进行了该方法的验证。所得到的方法参数(ZEN 回收率为 83%,重复性为 7.0%,再现性为 18%)符合委员会法规(EC)No 401/2006 的性能标准。开发的基于 RCHC-SPE 的 HPLC-FLD 方法允许对不同类型的食用植物油中的 ZEN 进行可靠定量,范围为 47-494μg/kg,也适用于基质可达的天然油。由于效率高,大大减少了基质负荷,有助于延长分析设备的使用寿命。此外,RCHC-SPE 小柱的可重复使用性有助于实现环保方法和降低分析成本。据我们所知,这是首次基于手动 RCHC-SPE 小柱报告食用植物油中 ZEN 的定量分析。由于其高性能,开发的 RCHC-SPE 方法是对现行欧洲标准方法 EN 16924:2017(HPLC-FLD 部分)的有前途的替代方法。
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