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基于肼的固相萃取和净化方法的开发及其在高效液相色谱荧光检测法中用于食用植物油中玉米赤霉烯酮的高选择性定量分析

Development of a Hydrazine-Based Solid-Phase Extraction and Clean-Up Method for Highly Selective Quantification of Zearalenone in Edible Vegetable Oils by HPLC-FLD.

机构信息

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.

出版信息

Toxins (Basel). 2022 Aug 11;14(8):549. doi: 10.3390/toxins14080549.


DOI:10.3390/toxins14080549
PMID:36006211
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9413969/
Abstract

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).

摘要

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。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/fa84/9413969/3a12ffcb2bef/toxins-14-00549-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/fa84/9413969/08a5f1e2991b/toxins-14-00549-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/fa84/9413969/674b714ebe56/toxins-14-00549-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/fa84/9413969/bda7613385bb/toxins-14-00549-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/fa84/9413969/3a12ffcb2bef/toxins-14-00549-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/fa84/9413969/08a5f1e2991b/toxins-14-00549-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/fa84/9413969/674b714ebe56/toxins-14-00549-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/fa84/9413969/bda7613385bb/toxins-14-00549-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/fa84/9413969/3a12ffcb2bef/toxins-14-00549-g004.jpg

相似文献

[1]
Development of a Hydrazine-Based Solid-Phase Extraction and Clean-Up Method for Highly Selective Quantification of Zearalenone in Edible Vegetable Oils by HPLC-FLD.

Toxins (Basel). 2022-8-11

[2]
Automated solid-phase extraction coupled online with HPLC-FLD for the quantification of zearalenone in edible oil.

Anal Bioanal Chem. 2015-5

[3]
Dynamic covalent hydrazine chemistry as a selective extraction and cleanup technique for the quantification of the Fusarium mycotoxin zearalenone in edible oils.

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[4]
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Anal Chim Acta. 2017-3-29

[5]
[Determination of zearalenone and α-zearalenol in vegetable oil and grain products by C_(18)-Al_2O_3 solid phase extraction column purification coupled with ultra-performance liquid chromatography tandem mass spectrometry].

Wei Sheng Yan Jiu. 2018-7

[6]
Simultaneous Determination of Aflatoxins and Benzo(a)pyrene in Vegetable Oils Using Humic Acid-Bonded Silica SPE HPLC-PHRED-FLD.

Toxins (Basel). 2022-5-18

[7]
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[8]
Molecularly imprinted vs. reversed-phase extraction for the determination of zearalenone: a method development and critical comparison of sample clean-up efficiency achieved in an on-line coupled SPE chromatography system.

Anal Bioanal Chem. 2018-2-17

[9]
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[10]
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引用本文的文献

[1]
Development of a Sensitive Enzyme Immunoassay Using Phage-Displayed Antigen-Binding Fragments for Zearalenone Detection in Cereal Samples.

Foods. 2025-2-22

[2]
Zearalenone, an estrogenic component, in bovine milk, amount and detection method; A systematic review and meta-analysis.

Toxicol Rep. 2024-7-4

[3]
Colorimetric and photothermal dual-mode immunosensor based on TiCT/AuNPs nanocomposite with enhanced peroxidase-like activity for ultrasensitive detection of zearalenone in cereals.

Mikrochim Acta. 2023-11-23

本文引用的文献

[1]
Research Progress of Safety of Zearalenone: A Review.

Toxins (Basel). 2022-6-2

[2]
Diet composition affects long-term zearalenone exposure on the gut-blood-liver axis metabolic dysfunction in mice.

Ecotoxicol Environ Saf. 2022-5-1

[3]
Analysis of Aflatoxins, Fumonisins, Deoxynivalenol, Ochratoxin A, Zearalenone, HT-2, and T-2 Toxins in Animal Feed by LC-MS/MS Using Cleanup with a Multi-Antibody Immunoaffinity Column.

J AOAC Int. 2022-9-6

[4]
Improved methods for biomarker analysis of the big five mycotoxins enables reliable exposure characterization in a population of childbearing age women in Rwanda.

Food Chem Toxicol. 2021-1

[5]
A mix-and-detect method based on colloidal gold immunochromatographic assay for on-site detection of zearalenone in edible oils.

Anal Methods. 2020-12-7

[6]
Zearalenone Removal from Corn Oil by an Enzymatic Strategy.

Toxins (Basel). 2020-2-13

[7]
Automated solid-phase extraction coupled online with HPLC-FLD for the quantification of zearalenone in edible oil.

Anal Bioanal Chem. 2015-5

[8]
Rapid determination of zearalenone in edible oils by HPLC with fluorescence detection.

Mycotoxin Res. 2009-7-9

[9]
Applications of reversible covalent chemistry in analytical sample preparation.

Analyst. 2012-9-26

[10]
Dynamic covalent hydrazine chemistry as a selective extraction and cleanup technique for the quantification of the Fusarium mycotoxin zearalenone in edible oils.

J Chromatogr A. 2010-2-18

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