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采用固相萃取-高效液相色谱-荧光检测法合成用于食品样品中黄曲霉毒素预富集的氧化石墨烯-二氧化硅/氧化锌/氧化亚铁纳米吸附剂。

Synthesis of GO-SiO/ZnO/FeO nano adsorbent for preconcentration of aflatoxins in food samples using SPE-HPLC-FLD method.

作者信息

Hosseini Hasan Ali, Sadat-Barati Mokhadare, Feizy Javad

机构信息

Department of Chemistry, Payame Noor University, 19395-4697 Tehran, Iran.

Department of Chemistry, Payame Noor University, 19395-4697 Tehran, Iran.

出版信息

Food Chem. 2025 Apr 1;470:142264. doi: 10.1016/j.foodchem.2024.142264. Epub 2024 Dec 19.

DOI:10.1016/j.foodchem.2024.142264
PMID:39755046
Abstract

This study demonstrates a new extraction method for determination of aflatoxins (AFs) in food samples by a GO-SiO/ZnO/FeO nanocomposite as new and effective sorbent. The nanocomposite structure was confirmed by FT-IR, XRD, EDX, FE-SEM, TEM, and mapping techniques. Optimization of the extraction process was conducted by investigating pH, adsorbent amount, sample volume, and solvent volume using central composite design (CCD). The method showed good linearity for AFs B, B, G, and G within specified ranges. Detection and quantification limits were 0.06-0.53 and 0.20-1.62 ng mL, respectively. The high performance liquid chromatography with fluorescence detector assisted by solid phase extraction (SPE-HPLC-FLD) method was applied to food samples, achieving recoveries of 70.15-97.08 %. Accuracy was confirmed through recovery measurements in spiked samples, with ranges of 70.15-97.85 % in wheat, 70.01-91.97 % in chickpeas, and 71.29-93.92 % in white pepper. Reusability and cost-effectiveness suggest its potential for preconcentration and determination of AFs in food samples.

摘要

本研究展示了一种新的提取方法,该方法使用新型高效吸附剂GO-SiO/ZnO/FeO纳米复合材料测定食品样品中的黄曲霉毒素(AFs)。通过傅里叶变换红外光谱(FT-IR)、X射线衍射(XRD)、能量散射X射线光谱(EDX)、场发射扫描电子显微镜(FE-SEM)、透射电子显微镜(TEM)和成像技术对纳米复合材料结构进行了确认。采用中心复合设计(CCD)研究pH值、吸附剂用量、样品体积和溶剂量,对提取过程进行了优化。该方法在规定范围内对AFs B1、B2、G1和G2显示出良好的线性。检测限和定量限分别为0.06 - 0.53 ng/mL和0.20 - 1.62 ng/mL。采用固相萃取-高效液相色谱-荧光检测法(SPE-HPLC-FLD)对食品样品进行分析,回收率为70.15% - 97.08%。通过对加标样品的回收率测量确认了准确性,小麦中的回收率范围为70.15% - 97.85%,鹰嘴豆中的回收率范围为70.01% - 91.97%,白胡椒中的回收率范围为71.29% - 93.92%。可重复使用性和成本效益表明其在食品样品中AFs预富集和测定方面具有潜力。

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