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首页> 美国卫生研究院文献>Toxins >Development and Validation of a LC-ESI-MS/MS Method for the Determination of Alternaria Toxins Alternariol Alternariol Methyl-Ether and Tentoxin in Tomato and Tomato-Based Products
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Development and Validation of a LC-ESI-MS/MS Method for the Determination of Alternaria Toxins Alternariol Alternariol Methyl-Ether and Tentoxin in Tomato and Tomato-Based Products

机译：液相色谱-ESI-MS / MS法测定番茄和番茄制品中的链霉菌毒素链烷醇甲醚和甲毒素的测定方法的建立和验证

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摘要

Alternaria species are capable of producing several secondary toxic metabolites in infected plants and in agricultural commodities, which play important roles in food safety. Alternaria alternata turn out to be the most frequent fungal species invading tomatoes. Alternariol (AOH), alternariol monomethyl ether (AME), and tentoxin (TEN) are some of the main Alternaria mycotoxins that can be found as contaminants in food. In this work, an analytical method based on liquid chromatography (LC) tandem mass spectrometry (MS/MS) detection for the simultaneous quantification of AOH, AME, and TEN in tomato and tomato-based products was developed. Mycotoxin analysis was performed by dispersive liquid-liquid microextraction (DLLME) combined with LC-ESI-MS/MS. Careful optimization of the MS/MS parameters was performed with an LC/MS system with the ESI interface in the positive ion mode. Mycotoxins were efficiently extracted from sample extract into a droplet of chloroform (100 µL) by DLLME technique using acetonitrile as a disperser solvent. Method validation following the Commission Decision No. 2002/657/EC was carried out by using tomato juice as a blank matrix. Limits of detection and quantitation were, respectively, in the range 0.7 and 3.5 ng/g. Recovery rates were above 80%. Relative standard deviations of repeatability (RSDr) and intermediate reproducibility (RSDR) were ≤ 9% and ≤ 15%, respectively, at levels of 25 and 50 ng/g. Five out of 30 analyzed samples resulted positive to at least one Alternaria toxin investigated. AOH was the most common Alternaria toxin found, but at levels close to LOQ (average content: 3.75 ng/g).
机译：链格孢属物种能够在受感染的植物和农产品中产生几种次生的有毒代谢产物，它们在食品安全中起着重要的作用。交链孢霉是入侵番茄的最常见真菌。交替糖（AOH），交替糖单甲醚（AME）和腱毒素（TEN）是一些主要的交替链霉菌真菌毒素，可作为食物中的污染物被发现。在这项工作中，开发了一种基于液相色谱（LC）串联质谱（MS / MS）检测的分析方法，用于同时定量番茄和番茄制品中的AOH，AME和TEN。通过与LC-ESI-MS / MS结合的分散液-液微萃取（DLLME）进行霉菌毒素分析。使用带有正离子模式下ESI接口的LC / MS系统对MS / MS参数进行了仔细的优化。通过使用乙腈作为分散剂的DLLME技术，从样品提取物中有效地提取霉菌毒素到一滴氯仿（100 µL）中。遵循委员会第2002/657 / EC号决定的方法验证是通过使用番茄汁作为空白基质进行的。检测限和定量限分别在0.7和3.5 ng / g范围内。回收率在80％以上。在25和50 ng / g的水平下，重复性（RSDr）和中间重复性（RSDR）的相对标准偏差分别≤9％和≤15％。 30个分析样品中有5个对所调查的至少一种链霉菌毒素呈阳性。 AOH是最常见的链格孢毒素，但含量接近LOQ（平均含量：3.75 ng / g）。

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