A fully automated method for simultaneous determination of aflatoxins and ochratoxin A in dried fruits by pressurized liquid extraction and online solid-phase extraction cleanup coupled to ultra-high-pressure liquid chromatography-tandem mass spectrometry
A fully automated method for simultaneous determination of aflatoxins and ochratoxin A in dried fruits by pressurized liquid extraction and online solid-phase extraction cleanup coupled to ultra-high-pressure liquid chromatography-tandem mass spectrometry
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DOI：
10.1007/s00216-015-8518-4
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发表时间：
2015-04-01
影响因子：
4.3
通讯作者：
Rastrelli, Luca
中科院分区：
文献类型：
--
作者：
Campone, Luca;Piccinelli, Anna Lisa;Rastrelli, Luca
根据当前食品安全的需求和发展前景，建立了一种快速、全自动的同时检测高风险食品--干果中毒性大、分布广的真菌毒素黄曲霉毒素（AFs）和赭曲霉毒素A（OTA）的分析方法。该方法基于在110 A ℃下用含水甲醇（30%）对浆状干果进行加压液体萃取（PLE），并用C18柱对PLE萃取物进行在线固相萃取（在线SPE）净化。采用超高压液相色谱-串联质谱法（UHPLC-MS/MS）对纯化后的样品进行直接分析，以灵敏、选择性地测定AFs和OTA。对不同干果（藤本水果、无花果和杏）的拟定分析方法进行了验证，方法检测限和定量限远低于欧盟法规规定的人类直接食用干果中AF和OTA的最大水平。此外，回收率（83- 103%）和重复性（RSD < 8，n = 3）符合欧盟法规要求的食品中霉菌毒素水平测定的性能标准。该方法的主要优点是整个分析过程的全自动化，减少了分析、样品操作和溶剂消耗的时间和成本，实现了高通量分析和高度准确和精确的结果。
According to current demands and future perspectives in food safety, this study reports a fast and fully automated analytical method for the simultaneous analysis of the mycotoxins with high toxicity and wide spread, aflatoxins (AFs) and ochratoxin A (OTA) in dried fruits, a high-risk foodstuff. The method is based on pressurized liquid extraction (PLE), with aqueous methanol (30 %) at 110 A degrees C, of the slurried dried fruit and online solid-phase extraction (online SPE) cleanup of the PLE extracts with a C18 cartridge. The purified sample was directly analysed by ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for sensitive and selective determination of AFs and OTA. The proposed analytical procedure was validated for different dried fruits (vine fruit, fig and apricot), providing method detection and quantification limits much lower than the AFs and OTA maximum levels imposed by EU regulation in dried fruit for direct human consumption. Also, recoveries (83-103 %) and repeatability (RSD < 8, n = 3) meet the performance criteria required by EU regulation for the determination of the levels of mycotoxins in foodstuffs. The main advantage of the proposed method is full automation of the whole analytical procedure that reduces the time and cost of the analysis, sample manipulation and solvent consumption, enabling high-throughput analysis and highly accurate and precise results.