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LC-FD 直接进样法检测葡萄牙葡萄酒中的赭曲霉毒素 A

Ochratoxin A survey in Portuguese wine by LC-FD with direct injection.

机构信息

Health Surveillance Group, Centre of Pharmaceutical Studies, Faculty of Pharmacy, University of Coimbra, Coimbra, Portugal.

出版信息

Talanta. 2010 Sep 15;82(4):1556-61. doi: 10.1016/j.talanta.2010.07.041. Epub 2010 Jul 24.

DOI:10.1016/j.talanta.2010.07.041
PMID:20801372
Abstract

Wine and grape juices were identified as one of the most important sources of ochratoxin A (OTA), a mycotoxin with diverse toxic effects that naturally appears in food and foodstuffs all over the world. The aim of this study was to assess the OTA levels in Portuguese wines through the application of a simple and accurate method based on liquid chromatography (LC) with direct injection, followed by fluorescence detection (FD). Randomly selected wine samples were used to evaluate the performance of direct injection as efficient, fast, inexpensive and safe sample preparation method. The proposed method was successfully validated. The limit of quantification (LOQ) was 1.0 microg/L and OTA recoveries from wine samples, spiked at the three fortification levels, were higher than 85.4%, with RSDs lower than 9.6% for both red and white wines. The presence of OTA was confirmed by methyl ester derivatization followed by LC analysis. Data on OTA levels were obtained for 60 Portuguese red and white wine samples. OTA was found in 12 samples, nine (26%) red wine samples and three (12%) white wine samples. Only one red wine sample and one white wine sample presented a contamination level above the LOQ, with 1.23 and 2.4 microg/L, respectively. It should be pointed out that this white wine sample exceeded the EC maximum permitted level of 2.0 microg/L. The safe dose established as 120 ng/kg body weight/week was not exceeded by the weekly intake estimated for the samples contaminated above the LOQ.

摘要

葡萄酒和葡萄汁被认为是赭曲霉毒素 A(OTA)的最重要来源之一,OTA 是一种具有多种毒性作用的真菌毒素,自然存在于世界各地的食品和食品中。本研究的目的是通过应用基于液相色谱(LC)的简单而准确的方法,直接进样,随后进行荧光检测(FD),评估葡萄牙葡萄酒中的 OTA 水平。随机选择葡萄酒样品来评估直接进样作为高效、快速、廉价和安全的样品制备方法的性能。所提出的方法得到了成功验证。定量限(LOQ)为 1.0μg/L,葡萄酒样品中 OTA 的回收率在三个加标水平下均高于 85.4%,对于红葡萄酒和白葡萄酒,RSD 均低于 9.6%。通过甲酯衍生化后进行 LC 分析,确认了 OTA 的存在。对 60 个葡萄牙红葡萄酒和白葡萄酒样品的 OTA 水平进行了检测。在 12 个样品中发现了 OTA,其中 9 个(26%)红葡萄酒样品和 3 个(12%)白葡萄酒样品。只有一个红葡萄酒样品和一个白葡萄酒样品的污染水平超过 LOQ,分别为 1.23μg/L 和 2.4μg/L。值得指出的是,该白葡萄酒样品超过了 EC 规定的 2.0μg/L 的最大允许水平。对于超过 LOQ 水平的样品,估计每周摄入量没有超过每周 120ng/kg 体重设定的安全剂量。

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