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还原氧化石墨烯修饰的 NiCo(OH) 纳米花用于涡旋辅助分散 µ-固相萃取婴幼儿食品谷物、大米和小麦粉中的有机磷农药。

Reduced graphene oxide decorated NiCo(OH) nanoflowers for vortexed assisted dispersive µ-solid-phase extraction of organophosphorus pesticides in baby food cereal, rice and wheat flour.

机构信息

Department of Chemistry, Faculty of Science, University of Jiroft, P. O. Box 7867161167, Jiroft, Iran.

Central Library, University of Jiroft, 7867161167, Jiroft, Iran.

出版信息

J Chromatogr A. 2024 Sep 27;1733:465277. doi: 10.1016/j.chroma.2024.465277. Epub 2024 Aug 15.

Abstract

Food safety is an important issue to protect humane health and improve the life quality. Hence, analysis of the possible contaminants in food samples is essential. A rapid and efficient vortexed-assisted dispersive µ-solid-phase extraction coupled with gas chromatography-mass spectrometry was proposed for simultaneous separation/preconcentration and determination of five commonly used organophosphorus pesticides. Reduced graphene oxide decorated NiCo(OH) nanoflowers as a novel nanostructure was synthetized and introduced for separation of the target pesticides from the wheat flour, rice flour, and baby food cereal samples. The characterization of the nanoflowers was accomplished by SEM-EDX, XRD, and FT-IR techniques. The main factors including pH, the amount of nanoflower, the volume of sample solution, salt concentration (ionic strength), desorption conditions (i.e. desorption solvent type and volume, and desorption time) on the pesticides extraction efficiencies were inquired using matrixed match method. Applying the optimum conditions, the linearity of 0.100-500.000 µg kg, LODs and LOQs in the range of 0.03-0.04 µg kg and 0.1 µg kg for the studied food samples were obtained. The repeatability (intra-day precision (n = 5)) of ≤ 2.0 % and reproducibility (inter-day precision, days = 5, n = 3) of ≤3.1 % and were appraise at three concentration levels (10, 50 and 100 μg kg of each analyte). High relative recoveries of 90.0-99.3 % ascertained high potential of the presented method for complex matrix analysis.

摘要

食品安全是保护人类健康和提高生活质量的重要问题。因此,分析食品样品中的可能污染物至关重要。本研究提出了一种快速高效的涡旋辅助分散μ-固相萃取结合气相色谱-质谱法,用于同时分离/预浓缩和测定五种常用的有机磷农药。合成了一种新型的纳米结构,即还原氧化石墨烯修饰的 NiCo(OH)纳米花,并将其用于从小麦粉、米粉和婴儿食品谷物样品中分离目标农药。采用 SEM-EDX、XRD 和 FT-IR 技术对纳米花进行了表征。采用矩阵匹配法考察了 pH 值、纳米花用量、样品溶液体积、盐浓度(离子强度)、解吸条件(解吸溶剂类型和体积、解吸时间)等主要因素对农药萃取效率的影响。在最佳条件下,对研究的食品样品进行测定,得到了 0.100-500.000 µg kg 的线性范围、0.03-0.04 µg kg 和 0.1 µg kg 的检出限和定量限。在三个浓度水平(每种分析物 10、50 和 100 µg kg)下,日内精密度(n = 5)重复性(≤2.0 %)和日间精密度(n = 3)重现性(≤3.1 %)良好。相对回收率为 90.0-99.3 %,表明该方法具有分析复杂基质的潜力。

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