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采用多免疫亲和柱净化和液相色谱荧光检测法测定土耳其传统浓缩果汁产品中的黄曲霉毒素和赭曲霉毒素A:单实验室验证

Determination of Aflatoxins and Ochratoxin A in Traditional Turkish Concentrated Fruit Juice Products by Multi-Immunoaffinity Column Cleanup and LC Fluorescence Detection: Single-Laboratory Validation.

作者信息

Kaymak Tugrul, Türker Levent, Tulay Hüseyin, Stroka Joerg

机构信息

Ankara Food Control Laboratory, 06170 Yenimahalle, Ankara, Turkey.

European Commission, Joint Research Centre, Directorate F - Health, Consumers, and Reference Materials, Retieseweg 111, 2400 Geel, Belgium.

出版信息

J AOAC Int. 2018 Nov 1;101(6):1839-1849. doi: 10.5740/jaoacint.17-0463. Epub 2018 Apr 27.

DOI:10.5740/jaoacint.17-0463
PMID:29703271
Abstract

: Pekmez and pestil are traditional Turkish foods made from concentrated grape juice, which can be contaminated with mycotoxins such as aflatoxins and ochratoxin A (OTA). : To carry out a single-laboratory validation of a method to simultaneously determine aflatoxins B, B₂, G, and G₂ and ochratoxin A in pekmez and pestil. : The homogenized sample is extracted with methanol-water (80 + 20) using a high-speed blender. The (sample) extract is filtered, diluted with phosphate-buffered saline solution, and applied to a multi-immunoaffinity column (AFLAOCHRA PREP®). Aflatoxins and ochratoxin A are removed with (neat) methanol and then directly analyzed by reversed-phase LC with fluorescence detection using post-column bromination (Kobra cell®). : Test portions of blank pekmez and pestil were spiked with a mixture of aflatoxins and ochratoxin A to give levels ranging from 2.6 to 10.4 μg/kg and 1.0-4.0 μg/kg, respectively. Recoveries for total aflatoxins and ochratoxin A ranged from 84 to 106% and 80-97%, respectively, for spiked samples. Based on results for spiked pekmez and pestil (30 replicates each at three levels), the repeatability RSD ranged from 1.6 to 12% and 2.7-11% for total aflatoxins and ochratoxin A, respectively. : The method performance in terms of recovery, repeatability, and detection limits has been demonstrated to be suitable for use as an Official Method. : First immunoaffinity column method validated for simultaneous analysis of aflatoxins and ochratoxin A in pekmez and pestil. Suitability for use for official purposes in Turkey, demonstrated by single-laboratory validation. Co-occurrence of aflatoxins and OTA in mulberry and carob pekmez reported for the first time.

摘要

佩克梅兹和佩斯蒂尔是用浓缩葡萄汁制成的传统土耳其食品,可能会被黄曲霉毒素和赭曲霉毒素A(OTA)等霉菌毒素污染。:对同时测定佩克梅兹和佩斯蒂尔中黄曲霉毒素B、B₂、G和G₂以及赭曲霉毒素A的方法进行单实验室验证。:将匀浆后的样品用高速搅拌器以甲醇 - 水(80 + 20)提取。(样品)提取物经过过滤,用磷酸盐缓冲盐溶液稀释,然后应用于多免疫亲和柱(AFLAOCHRA PREP®)。黄曲霉毒素和赭曲霉毒素A用(纯)甲醇洗脱,然后直接通过反相液相色谱结合柱后溴化荧光检测法(Kobra cell®)进行分析。:空白佩克梅兹和佩斯蒂尔的测试部分分别添加黄曲霉毒素和赭曲霉毒素A的混合物,使其含量范围分别为2.6至10.4μg/kg和1.0 - 4.0μg/kg。加标样品中总黄曲霉毒素和赭曲霉毒素A的回收率分别为84%至106%和80 - 97%。根据加标佩克梅兹和佩斯蒂尔的结果(每个水平各30次重复),总黄曲霉毒素和赭曲霉毒素A的重复性相对标准偏差分别为1.6%至12%和2.7 - 11%。:该方法在回收率、重复性和检测限方面的性能已被证明适用于作为官方方法使用。:首次验证了用于同时分析佩克梅兹和佩斯蒂尔中黄曲霉毒素和赭曲霉毒素A的免疫亲和柱方法。通过单实验室验证证明了其在土耳其官方用途的适用性。首次报道了桑椹和角豆佩克梅兹中黄曲霉毒素和OTA的共存情况。

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