Ghorbani Mahdi, Keshavarzi Majid, Pakseresht Maryam, Mohammadi Parisa, Shams Alireza, Mehraban Abouzar, Ismailzadeh Amir
Razi Research Center, Khorasan Razavi Education, Mashhad, Iran.
Department of Pharmacodynamics and Toxicology, School of Pharmacy, Mashhad University of Medical Sciences, Mashhad, Iran.
Anal Bioanal Chem. 2023 Sep;415(23):5681-5694. doi: 10.1007/s00216-023-04842-0. Epub 2023 Jul 29.
Aflatoxins (AFs), an important category of pollutants, are formed in many foods and adversely affect human health. Therefore, their determination is critical to ensuring human food health. An efficient dispersive solid-phase microextraction technique was developed as a simple and straightforward sample preparation technique for determination of four aflatoxins using a high-performance liquid chromatography (HPLC) fluorescence detector. A novel efficient, green sorbent for extracting AFs was synthesized based on hydrothermal and chemical strategies. The amounts of three sorbent components were optimized using a mixture design (simplex lattice design), including 14 experiments. The optimal amount of amino-bimetallic Fe/Ni-MIL-53 nanospheres, chitosan, and magnetic FeO nanoparticles as sorbent components was 0.87, 0.67, and 0.47 g, respectively. Also, various factors affecting the process of AF determination were studied and optimized in two successive experimental designs, including the definitive screening design and the Box-Behnken design. Under optimal conditions, the linear ranges for measuring aflatoxin B1, aflatoxin B2, aflatoxin G1, and aflatoxin G2 were 0.05-82.6, 0.07-86.4, 0.08-85.7, and 0.07-89.5 ng mL, respectively. The relative standard deviations under inter-day and intra-day conditions for measuring AFs at three analyte concentrations were determined in triplicate analysis and were in the ranges of 3.7-4.6% and 4.9-6.1% for water sample analysis, respectively. The qualitative detection limits for determining AFs were between 0.01 and 0.05 ng mL. The pre-concentration factor of the method for measuring AFs ranged from 739.7 to 802.1. The proposed method was used for determining AFs in several real samples, including herbal distillate, black tea, corn, and real water samples. The relative recovery and standard deviation were 87.8-97.8% and 4.10-6.82%, respectively.
黄曲霉毒素（AFs）是一类重要的污染物，在许多食品中形成并对人体健康产生不利影响。因此，对其进行测定对于确保人类食品安全至关重要。本文开发了一种高效的分散固相微萃取技术，作为一种简单直接的样品制备技术，用于使用高效液相色谱（HPLC）荧光检测器测定四种黄曲霉毒素。基于水热和化学策略合成了一种新型高效、绿色的黄曲霉毒素萃取吸附剂。使用混合设计（单纯形格子设计）对三种吸附剂成分的用量进行了优化，共进行了14次实验。作为吸附剂成分的氨基双金属Fe/Ni-MIL-53纳米球、壳聚糖和磁性FeO纳米颗粒的最佳用量分别为0.87、0.67和0.47 g。此外，在两个连续的实验设计中，包括确定性筛选设计和Box-Behnken设计，研究并优化了影响黄曲霉毒素测定过程的各种因素。在最佳条件下，测定黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1和黄曲霉毒素G2的线性范围分别为0.05 - 82.6、0.07 - 86.4、0.08 - 85.7和0.07 - 89.5 ng/mL。在三个分析物浓度下，对水样进行日间和日内条件下测定黄曲霉毒素的相对标准偏差在三次重复分析中分别为3.7 - 4.6%和4.9 - 6.1%。测定黄曲霉毒素的定性检测限在0.01至0.05 ng/mL之间。该方法测定黄曲霉毒素的预富集因子范围为739.7至802.1。所提出的方法用于测定几种实际样品中的黄曲霉毒素，包括草药提取物、红茶、玉米和实际水样。相对回收率和标准偏差分别为87.8 - 97.8%和4.10 - 6.82%。
