Abstract：
UPLC-MS/MS analytical conditions for the analysis of aflatoxins in spices were optimized and validated in this study. Liquid-liquid partition-based protocols for the cleaning up of extracts using common organic solvents such as acetonitrile, hexane, and ethyl acetate were developed and validated. The developed liquid-liquid partition methods were compared with immuno-affinity column and QuEChERS clean-up methods for the UPLC-MS/MS analysis of aflatoxins in 8 spices. The reduction of lipophilic components using the partition with hexane is particularly useful in spices like red pepper that have higher levels of fatty acids, carotenoids, sterols, triterpenoids, etc. The subsequent partitioning with ethyl acetate considerably reduced the matrix interference from the polar components and increased the sensitivity. The cleaning up of spice extracts using liquid-liquid partition techniques resulted in limits of quantification (LOQ) of 2-5 µgL-1 in UPLC-MS/MS analysis. Trueness, repeatability, and reproducibility of the methods were in acceptable ranges. The accuracy of the developed methods was further verified by analyzing aflatoxins in naturally incurred samples of spices and comparing the results with those obtained from the immuno-affinity column cleanup-HPLC-FD method.
摘要：
本研究对香料中黄曲霉毒素的UPLC-MS/MS分析条件进行了优化和验证。基于液-液分配的方案，用于使用常见的有机溶剂（如乙腈）清洁提取物，己烷,和乙酸乙酯进行了开发和验证。将开发的液-液分配方法与免疫亲和柱和QuEChERS净化方法进行了比较，以对8种香料中的黄曲霉毒素进行UPLC-MS/MS分析。使用己烷分区减少亲脂性成分在香料中特别有用，如红辣椒，脂肪酸含量较高，类胡萝卜素，固醇,三萜类，等。随后的乙酸乙酯分配大大减少了极性成分的基质干扰，并提高了灵敏度。使用液-液分配技术清洁香料提取物导致UPLC-MS/MS分析中2-5µgL-1的定量限（LOQ）。Trueness,重复性,方法的可重复性在可接受的范围内。通过分析天然产生的香料样品中的黄曲霉毒素并将结果与从免疫亲和柱清理-HPLC-FD方法获得的结果进行比较，进一步验证了所开发方法的准确性。
