Development and validation of extraction and clean-up procedures for UPLC-MS/MS analysis of aflatoxins in spices.

IF 2.6 4区医学 Q2 MYCOLOGY Mycotoxin Research Pub Date : 2024-11-01 Epub Date: 2024-07-11 DOI:10.1007/s12550-024-00546-1

Ranjith Arimboor, Venugopal Gopalan, Srilatha C M, Remashree Azhimala Bhaskaranpillai

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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.

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开发和验证用于 UPLC-MS/MS 分析香料中黄曲霉毒素的提取和净化程序。

本研究优化并验证了用于分析香料中黄曲霉毒素的 UPLC-MS/MS 分析条件。开发并验证了使用乙腈、正己烷和乙酸乙酯等常见有机溶剂对提取物进行净化的液液分配法。在对 8 种香料中的黄曲霉毒素进行 UPLC-MS/MS 分析时，将所开发的液液分配法与免疫亲和柱和 QuEChERS 净化法进行了比较。使用正己烷分配法减少亲脂性成分的含量，尤其适用于红辣椒等脂肪酸、类胡萝卜素、甾醇、三萜类化合物含量较高的香料。随后用乙酸乙酯分馏可大大减少极性成分对基质的干扰，提高灵敏度。使用液液分配技术对香料提取物进行净化后，UPLC-MS/MS 分析的定量限 (LOQ) 为 2-5 µgL-1。方法的真实性、重复性和再现性均在可接受的范围内。通过分析自然产生的香料样品中的黄曲霉毒素，并将结果与免疫亲和柱净化-高效液相色谱-荧光定量分析方法得出的结果进行比较，进一步验证了所开发方法的准确性。

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来源期刊

Mycotoxin Research MYCOLOGYTOXICOLOGY-TOXICOLOGY

CiteScore

6.40

自引率

6.70%

发文量

期刊介绍： Mycotoxin Research, the official publication of the Society for Mycotoxin Research, is a peer-reviewed, scientific journal dealing with all aspects related to toxic fungal metabolites. The journal publishes original research articles and reviews in all areas dealing with mycotoxins. As an interdisciplinary platform, Mycotoxin Research welcomes submission of scientific contributions in the following research fields: - Ecology and genetics of mycotoxin formation - Mode of action of mycotoxins, metabolism and toxicology - Agricultural production and mycotoxins - Human and animal health aspects, including exposure studies and risk assessment - Food and feed safety, including occurrence, prevention, regulatory aspects, and control of mycotoxins - Environmental safety and technology-related aspects of mycotoxins - Chemistry, synthesis and analysis.