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采用超高效液相色谱-高分辨质谱联用分析谷物中镰刀菌毒素的新方法。

Novel approaches in analysis of Fusarium mycotoxins in cereals employing ultra performance liquid chromatography coupled with high resolution mass spectrometry.

机构信息

Institute of Chemical Technology, Faculty of Food and Biochemical Technology, Department of Food Chemistry and Analysis, Technicka 3, 166 28 Prague 6, Czech Republic.

出版信息

Anal Chim Acta. 2010 Mar 3;662(1):51-61. doi: 10.1016/j.aca.2009.12.034. Epub 2010 Jan 13.

Abstract

Rapid, simple and cost-effective analytical methods with performance characteristics matching regulatory requirements are needed for effective control of occurrence of Fusarium toxins in cereals and cereal-based products to which they might be transferred during processing. Within this study, two alternative approaches enabling retrospective data analysis and identification of unknown signals in sample extracts have been implemented and validated for determination of 11 major Fusarium toxins. In both cases, ultra-high performance liquid chromatography (U-HPLC) coupled with high resolution mass spectrometry (HR MS) was employed. (13)C isotopically labeled surrogates as well as matrix-matched standards were employed for quantification. As far as time of flight mass analyzer (TOF-MS) was a detection tool, the use of modified QuEChERS (quick easy cheap effective rugged and safe) sample preparation procedure, widely employed in multi-pesticides residue analysis, was shown as an optimal approach to obtain low detection limits. The second challenging alternative, enabling direct analysis of crude extract, was the use of mass analyzer based on Orbitrap technology. In addition to demonstration of full compliance of the new methods with Commission Regulation (EC) No. 401/2006, also their potential to be used for confirmatory purposes according to Commission Decision 2002/657/EC has been critically assessed.

摘要

需要快速、简单且具有成本效益的分析方法,并且其性能特征要与法规要求相匹配,以有效控制谷物和可能在加工过程中转移到这些谷物制品中的真菌毒素的出现。在本研究中,已经实施并验证了两种替代方法,以实现对 11 种主要镰刀菌毒素的回溯数据分析和未知信号的识别。在这两种情况下,均采用超高效液相色谱(U-HPLC)与高分辨率质谱(HR-MS)联用。(13)C 同位素标记的内标物以及基质匹配标准品用于定量。由于飞行时间质谱仪(TOF-MS)是一种检测工具,因此,已显示出使用广泛应用于多种农药残留分析的改良 QuEChERS(快速、简便、廉价、有效、坚固和安全)样品制备程序是获得低检测限的最佳方法。另一种具有挑战性的替代方法是使用基于轨道阱技术的质量分析器,能够直接分析粗提物。除了证明新方法完全符合委员会法规(EC)No.401/2006 之外,还根据委员会决定 2002/657/EC 对其用于确证目的的潜力进行了严格评估。

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