使用免疫亲和柱净化、柱后衍生化和带荧光检测的液相色谱法测定橄榄油、花生油和芝麻油中的黄曲霉毒素B1、B2、G1和G2：2013年5月首次行动

Determination of aflatoxins B1, B2, G1, and G2 in olive oil, peanut oil, and sesame oil using immunoaffinity column cleanup, postcolumn derivatization, and liquid chromatography with fluorescence detection: first action 2013.05.

作者信息

Bao Lei, Liang Chengzhu, Trucksess Mary W, Xu Yanli, Lv Ning, Wu Zhenxing, Jing Ping, Fry Fred S

机构信息

Shandong Exit-Entry Inspection and Quarantine Bureau of China, Qing Dao, China 266002.

出版信息

J AOAC Int. 2013 Sep-Oct;96(5):1017-8. doi: 10.5740/jaoacint.13-129.

DOI:10.5740/jaoacint.13-129

PMID:24282940

Abstract

A collaborative study of a method for determination of aflatoxins (AFs) B1, B2, G1, and G2 in olive oil, peanut oil, and sesame oil using immunoaffinity column cleanup, postcolumn derivatization, and LC with fluorescence detection, previously published in J. AOAC Int. 95, 1689-1700 (2012), was approved as First Action 2013.05 on March 29, 2013 by the Method-Centric Committee for Aflatoxins in Edible Oils. The method uses methanol for extraction followed by filtration. The extract is applied to an immunoaffinity column with antibodies specific for AFs, which are then eluted from the column with a methanol solution. Determination and quantification occur using RP-LC with fluorescence detection after postcolumn derivatization. The average recovery of AFs in olive, peanut, and sesame oils in spiked samples (levels between 2.0 and 20.0 microg/kg) ranged from 84 to 92%. The recoveries for AFs B1, B2, G1, and G2 were 86-93, 89-95, 85-97, and 76-85%, respectively. Within-laboratory RSD (RSDr) values for AFs ranged from 3.4 to 10.2%. RSDr values forAF B1, B2, G1, and G2 were 3.5-10.9, 3.2-9.5, 6.5-14.9, and 4.8-14.2%, respectively. Between-laboratory RSD (RSDR) values for AFs were 6.1-14.5%. RSD, values for AFs B1, B2, G1, and G2 were 7.5-15.4, 7.1-14.6, 10.8-18.1, and 7.6-23.7%, respectively. Horwitz ratio values were < or =2 for the analytes in the three matrixes.

摘要

一项关于使用免疫亲和柱净化、柱后衍生化和带荧光检测的液相色谱法测定橄榄油、花生油和芝麻油中黄曲霉毒素（AFs）B1、B2、G1和G2的协作研究，此前发表于《美国分析化学家协会国际期刊》95, 1689 - 1700 (2012)，于2013年3月29日被食用油中黄曲霉毒素以方法为中心委员会批准为2013.05首次行动。该方法使用甲醇进行萃取，随后过滤。提取物应用于对AFs具有特异性抗体的免疫亲和柱，然后用甲醇溶液从柱上洗脱。柱后衍生化后，使用带荧光检测的反相液相色谱法进行测定和定量。加标样品（水平在2.0至20.0微克/千克之间）中橄榄油、花生油和芝麻油中AFs的平均回收率在84%至92%之间。AFs B1、B2、G1和G2的回收率分别为86 - 93%、89 - 95%、85 - 97%和76 - 85%。AFs在实验室内的相对标准偏差（RSDr）值在3.4%至10.2%之间。AF B1、B2、G1和G2的RSDr值分别为3.5 - 10.9%、3.2 - 9.5%、6.5 - 14.9%和4.8 - 14.2%。AFs在实验室间的相对标准偏差（RSDR）值为6.1 - 14.5%。AFs B1、B2、G1和G2的RSDR值分别为7.5 - 15.4%、7.1 - 14.6%、10.8 - 18.1%和7.6 - 23.7%。三种基质中分析物的霍维茨比值≤2。