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利用裸 Fe3O4 作为磁性吸附剂结合高效液相色谱-荧光检测法快速灵敏检测植物油中的黄曲霉毒素 B1、B2、G1 和 G2。

Rapid and Sensitive Detection of Aflatoxin B1, B2, G1 and G2 in Vegetable Oils Using Bare Fe3O4 as Magnetic Sorbents Coupled with High-Performance Liquid Chromatography with Fluorescence Detection.

机构信息

Institute of Agricultural Quality Standards and Testing Technology Research, Hubei Academy of Agricultural Science/Hubei Key Laboratory of Nutritional Quality and Safety of Agro products, Wuhan 430064, Hubei, China.

School of Chemistry and Materials Engineering, Liupanshui Normal University, Liupanshui 553004, Guizhou, China.

出版信息

J Chromatogr Sci. 2020 Jul 24;58(7):678-685. doi: 10.1093/chromsci/bmaa026.

DOI:10.1093/chromsci/bmaa026
PMID:32548633
Abstract

This paper reports a simple, sensitive and reliable method for the simultaneous detection of aflatoxin B1, B2, G1 and G2 in vegetable oils. Aflatoxins were extracted by magnetic solid phase extraction followed by high-performance liquid chromatography, then postcolumn photochemical derivatization and finally detected by fluorescence detector. Vegetable oil samples were first diluted with hexane and then commercial bare Fe3O4 nanoparticles were directly employed as sorbents to extract aflatoxins from complex vegetable oil samples, which significantly simplified the procedure of sample preparation and largely improved the sample analysis throughput. The effects of various parameters such as the amount of sorbent, loading, washing and eluting conditions were carefully optimized to improve the extraction efficiencies of aflatoxins. Under the optimal conditions, the limits of detection of four aflatoxins ranged from 0.01 μg/kg to 0.16 μg/kg, and squared regression coefficients (R2) >0.9990 were obtained within the linear range of 0.1-20 μg/kg (except for aflatoxin G2 with 0.5-20 μg/kg). Furthermore, the recoveries spiked at four concentration levels in a blank vegetable oil sample were from 82.6 to 106.2%, with inter- and intraday relative standard deviations <9.8%, indicating good accuracy and precision of the proposed method.

摘要

本文报道了一种用于同时检测植物油中黄曲霉毒素 B1、B2、G1 和 G2 的简单、灵敏、可靠的方法。黄曲霉毒素通过磁固相萃取提取,然后进行高效液相色谱分析,再进行柱后光化学反应衍生化,最后用荧光检测器检测。首先将植物油样品用正己烷稀释,然后直接使用商业裸 Fe3O4 纳米粒子作为吸附剂从复杂的植物油样品中提取黄曲霉毒素,这大大简化了样品制备的步骤,大大提高了样品分析的通量。仔细优化了各种参数,如吸附剂的用量、加载、洗涤和洗脱条件,以提高黄曲霉毒素的提取效率。在最佳条件下,四种黄曲霉毒素的检测限范围为 0.01μg/kg 至 0.16μg/kg,在 0.1-20μg/kg 的线性范围内(除黄曲霉毒素 G2 的 0.5-20μg/kg 外),均获得了平方回归系数(R2)>0.9990。此外,在空白植物油样品中四个浓度水平的加标回收率为 82.6%至 106.2%,日内和日间相对标准偏差<9.8%,表明该方法具有良好的准确性和精密度。

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