现行黄曲霉毒素液相色谱检测法的比较与评价

Comparison and assessment of aflatoxins determination by ultra-pressure liquid chromatography

中文关键词:  三氟乙酸(TFA)  光化学柱后衍生  大体积流动池  黄曲霉毒素  液相色谱

英文关键词:trifluoroacetic acid(TFA)  photochemical post column derivation  large volume flow cell  aflatoxin  liquid chromatography

中文摘要:

      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。

英文摘要:

      Objective To compare and evaluate several methods for determination of aflatoxins by ultra-pressure liquid chromatography (UPLC) combined with fluorescence detection (FLD). Methods Samples were extracted by homogeneity (vortex) and ultrasound-assisted liquid-liquid extraction, and purified by im-munoaffinity column and multifunctional column. Then the analytes were analysed by UPLC-FLD with trifluoroacetic acid (TFA) pre-column derivation, photochemical post column derivation, iodine and bromine post column derivation, large volume flow cell and photochemical post column derivation tandem large volume flow cell. Results The results showed each method was satisfying, and each method could fulfill the inspection requirements of common samples. Conclusion The method of UPLC combined with fluorescence detector and large volume flow cell had the highest sensitivity among these methods. This method could not only raise the work efficiency, but also reduce a lot of poisonous and harmful organic solvent. Meanwhile, the method successfully fulfilled the minimum limiting level requests according to the GB 2761-2011. Both acetonitrile aqueous solution and methanol aqueous solution could extract the aflatoxins from samples successfully. And the cleanup effect of immunoaffinity column achieved better results than that of multifunctional column.