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目的综合评价检测黄曲霉毒素的几种现行液相色谱-荧光法。方法采用均质(涡旋)、超声辅助液液萃取技术对样品中的黄曲霉毒素进行提取,免疫亲和柱和多功能柱净化。并采用不同的检测技术[三氟乙酸(TFA)柱前衍生法、光化学柱后衍生法、碘和溴柱后衍生法、大体积流动池直接检测及光化学柱后衍生串联大体积流动池]对玉米质控样品中黄曲霉毒素进行了分析。结果各方法的检测结果均较理想,可满足常规样品的检测要求。结论超高压液相色谱-大体积流动池检测法在有效提高工作效率的同时,大量减少了有毒有害试剂的使用量,且具有最高的检测灵敏度,可满足GB 2761-2011中对各类样品中黄曲霉毒素的限量要求。采用乙腈-水或甲醇-水体系均能达到较好提取黄曲霉毒素的目的。免疫亲和柱的净化效果较多功能柱好。
Objective To synthetically evaluate several current liquid chromatography-fluorescence methods for the detection of aflatoxins. Methods The aflatoxins in the samples were extracted by homogenization (vortex) and sonication-assisted liquid-liquid extraction, and purified by immunoaffinity column and multi-functional column. And different detection techniques [trifluoroacetic acid (TFA) pre-column derivatization, photochemical post-column derivatization, iodine and bromine post-column derivatization, direct detection of large volume flow cell and tandem large-volume flow cell of photochemical post- Aflatoxins in corn quality control samples were analyzed. Results The results of each method were satisfactory, which can meet the testing requirements of routine samples. Conclusion Ultra-high pressure liquid chromatography - large-volume flow cell detection method in an effective manner to improve work efficiency, while reducing the use of toxic and harmful reagents, and has the highest detection sensitivity to meet the GB 2761-2011 in a variety of samples Aflatoxin limited requirements. The use of acetonitrile - water or methanol - water system can achieve a better extraction aflatoxin purposes. Immune affinity column purification effect more functional column.