摘要
目的建立粮油食品中4种黄曲霉毒素AFG1,AFB1,AFG2,AFB2的免疫亲和柱净化,柱前衍生高效液相色谱-荧光检测法。方法样品经甲醇-水（70＋30）超声提取30 min后,提取液用定性滤纸过滤,然后吸取一定量的提取液稀释后用免疫亲和柱净化,收集一定量的甲醇洗脱液于衍生瓶中,60℃条件下氮吹仪吹干,再用正己烷和三氟乙酸在40℃条件下衍生15 min后氮吹仪吹干,然后用水＋甲醇（45＋55）溶解,C18色谱柱分离,高效液相色谱-荧光检测器测定,外标法定量。结果在优化条件下,4种黄曲霉毒素的分离效果良好,AFG1,AFB1,AFG2,AFB2的检出限分别为0.03μg/kg、0.03μg/kg、0.01μg/kg、0.01μg/kg,回收率为81.9%～97.6%,80.7%～98.3%,57.6%～80.3%,69.3%～106.4%,RSD均低于4.8%。结论该方法简单、快速、灵敏、准确、重现性好,可满足粮油食品中黄曲霉毒素AFG1,AFB1,AFG2,AFB2检测的需要。
Objective A method for determination of aflatoxin B1 , B2, G,, G2 by cleaning up immunoaffinity column and HPLC with pre - column derivatization was developed. Methods The samples were extracted by ultrasonic treatment with methanol - water solution （70 ± 30） for 30 min, then the extract liquor was filtered by qualitative filter paper, and a certain vol- ume of filtrate was diluted with water, cleaned up by immunoaffinity column. The eluent was dried by nitrogen blowing concen- trator in a bottle, after that, derived with n -hexane and trifluoroacetic acid （TFA） at 40 ~C by 15 min, then dried by nitrogen blowing concentrator again. Before C,s chromatographic column separation, the analytes were dissolved with methanol - water so- lution （55 ＋ 45）. After separation, aflatoxins were determinated by fluorescence detector. Results Under optimize conditions, four kinds of aflatoxins were separated very well, the limits of detection of aflatoxin B1, B2, G1, G2 were 0. 03μg/kg, 0.03 μg/kg,O. 01 μg/kg,0. 01μg/kg respectively, and the recoveries of analytes were 81.9% - 97.6% ,80.7% - 98.3%, 57.6% - 80.3% ,69.3% - 106.4%, and RSD were all below 4.8%. Conclusion The method is simple, rapid, sensitive, accurate and with good repeatability, which is suitable for the determination of aflatoxin B1 , B2, G1 , G2 in grain and oil foods.
出处
《中国卫生检验杂志》
北大核心
2014年第17期2477-2480,共4页
Chinese Journal of Health Laboratory Technology
