College of Chemical Engineering, Zhejiang University of Technology, Zhejiang, China.
Lab of Physicochemical Research, Department of Physicochemical & Toxicology, Zhejiang Provincial Center for Disease Control and Prevention, Zhejiang, China.
J Sep Sci. 2017 May;40(10):2141-2150. doi: 10.1002/jssc.201601326. Epub 2017 Apr 19.
A novel pre-treatment was proposed for the simultaneous determination of aflatoxins, ochratoxin A and zearalenone in foodstuffs using high-performance liquid chromatography with fluorescence detection. The analytical procedure was based on a first step using a quick, easy, cheap, effective, rugged, and safe based extraction procedure, followed by salting out and purification with a C solid-phase extraction column as interference removal clean-up. Subsequently, collected supernatant was subjected to dispersive liquid-liquid microextraction. Response surface methodology based on central composite design was employed to optimize conditions in the microextraction procedure. Under the optimum conditions, satisfactory analytical performance with recoveries ranging from 63.22 to 107.6% were achieved in different types of cereals and beans, as well as desirable precisions (0.81-8.13%). Limits of detections and quantifications for these six mycotoxins ranging from 0.03 to 13 μg/kg and 0.22 to 44 μg/kg, respectively, were obtained. Finally, the established method was successfully validated by four certified reference materials (P = 0.897 > 0.05) and applied to 79 samples from local markets.
提出了一种新的前处理方法,用于同时测定食品中的黄曲霉毒素、赭曲霉毒素 A 和玉米赤霉烯酮。该分析方法基于第一步骤使用快速、简单、廉价、有效、坚固和安全的基于提取程序,然后用 C 固相萃取柱进行盐析和净化以去除干扰物。随后,收集上清液进行分散液液微萃取。采用基于中心复合设计的响应面法优化微萃取程序的条件。在最佳条件下,在不同类型的谷物和豆类中,回收率在 63.22%至 107.6%之间,获得了令人满意的分析性能,以及良好的精密度(0.81-8.13%)。这些六种真菌毒素的检测限和定量限分别为 0.03 至 13μg/kg 和 0.22 至 44μg/kg。最后,通过四个认证参考物质(P=0.897>0.05)对建立的方法进行了验证,并应用于当地市场的 79 个样品。