Rapid analysis of aflatoxins B1, B2, and ochratoxin A in rice samples using dispersive liquid-liquid microextraction combined with HPLC
Rapid analysis of aflatoxins B1, B2, and ochratoxin A in rice samples using dispersive liquid-liquid microextraction combined with HPLC
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DOI：
10.1002/jssc.201300970
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发表时间：
2014-01-01
影响因子：
3.1
通讯作者：
Liu, Cheng-Lan
中科院分区：
文献类型：
--
作者：
Lai, Xian-Wen;Sun, Dai-Li;Liu, Cheng-Lan
建立了分散液液微萃取-液相色谱-荧光检测法测定大米中黄曲霉毒素B-1、黄曲霉毒素B-2和赭曲霉毒素A的新方法。大米样品用乙腈/水/乙酸混合液提取后，通过分散液-液微萃取将霉菌毒素快速分配到小体积的有机溶剂（氯仿）中。黄曲霉毒素B-1和B-2经柱前衍生化后，采用液相色谱荧光检测法同时测定3种霉菌毒素。对影响萃取和分散液-液微萃取过程的参数进行了优化，包括萃取溶剂、萃取剂的种类和体积、分散溶剂的体积、盐的加入量、pH值和萃取时间。优化方案提供了约1.25的富集因子，检测限（0.06-0.5 g/kg）低于现行法规规定的黄曲霉毒素和赭曲霉毒素A的最高水平。三种霉菌毒素的平均回收率为82.9- 112%，所有情况下的RSD均小于7.9%。该方法已成功地应用于从中国当地超市收集的商品大米样品中的霉菌毒素的测定。
A novel, simple, and rapid method is presented for the analysis of aflatoxin B-1, aflatoxin B-2, and ochratoxin A in rice samples by dispersive liquid-liquid microextraction combined with LC and fluorescence detection. After extraction of the rice samples with a mixture of acetonitrile/water/acetic acid, mycotoxins were rapidly partitioned into a small volume of organic solvent (chloroform) by dispersive liquid-liquid microextraction. The three mycotoxins were simultaneously determined by LC with fluorescence detection after precolumn derivatization for aflatoxin B-1 and B-2. Parameters affecting both extraction and dispersive liquid-liquid microextraction procedures, including the extraction solvent, the type and volume of extractant, the volume of dispersive solvent, the addition of salt, the pH and the extraction time, were optimized. The optimized protocol provided an enrichment factor of approximately 1.25 and with detection of limits (0.06-0.5 g/kg) below the maximum levels imposed by current regulations for aflatoxins and ochratoxin A. The mean recovery of three mycotoxins ranged from 82.9-112%, with a RSD less than 7.9% in all cases. The method was successfully applied to measure mycotoxins in commercial rice samples collected from local supermarkets in China.