Determination of strobilurin fungicides residual in vegetables based on amino modified magnetic graphene oxide solid phase extraction coupled with GC–MS/MS

IF 3.8 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Journal of Chromatography A Pub Date : 2024-11-07 DOI:10.1016/j.chroma.2024.465455
Qinghua Yang , Qianying Qiu , Yilan Shi , Jinxin Wang , Feng Chen , Juan Yang , Weibing Zhang , Zhen Yin
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Abstract

This research investigated the creation and utilization of an amino-functionalized magnetic graphene oxide (Fe₃O₄-NH₂@GO) nanocomposite as a selective sorbent for extracting and identifying strobilurin fungicides (SFs) from vegetable samples. The investigation utilized a method where magnetic solid phase extraction (MSPE) was integrated with Gas chromatography-triple quadrupole mass spectrometer (GC–MS/MS) for analysis. The physicochemical properties of synthesized sorbent were characterized using Scanning electron microscope (SEM) , Fourier infrared transform spectrum (FT-IR) , X Ray Diffraction (XRD), and vibrating sample magnetometry (VSM) techniques. The adsorption performance of Fe₃O₄-NH₂@GO aligned with the pseudo-second-order kinetics, Elovich, and Freundlich isothermal adsorption models, suggesting various interactions with SFs, including π-π interactions, hydrogen bonding, and electrostatic forces. The maximum adsorption capacity of two selected representative SFs (Picoxystrobin and E-metominostrobin) for the adsorbent were 55.85 mg/g and 47.35 mg/g, respectively. Additionally, the amino group exhibited notable potential for SFs adsorption. Parameters for MSPE, such as the quantity of sorbent, adsorption duration, eluent types and volumes, and sample pH, were optimized. Under optimal conditions, the developed method showed satisfactory performance within a range of 10 to 2000 µg L⁻¹ (R² ≥ 0.9969), low detection limits (0.01–0.080 µg/kg), high analyte recovery (80.5–104.3 %), and good precision (RSD ≤ 4.96 %, n = 6). This method is rapid, straightforward, environmentally friendly, demonstrates good sensitivity and providing a new perspectives on developing sorbents for SFs in complex food matrices. Also Fe₃O₄-NH₂@GO as a sorbent firstly used for extraction and enrichment of phenyl fungicides residues in food samples exhibits remarkable promise, thereby contributing to the advancement of pesticides residue determination methodologies.
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基于氨基修饰的磁性氧化石墨烯固相萃取-气相色谱-质谱联用技术测定蔬菜中的残留杀菌剂。
本研究调查了氨基功能化磁性氧化石墨烯(Fe₃O₄-NH₂@GO)纳米复合材料作为选择性吸附剂在蔬菜样品中提取和鉴定杀菌剂(SFs)中的应用。研究采用磁性固相萃取(MSPE)与气相色谱-三重四极杆质谱仪(GC-MS/MS)相结合的方法进行分析。利用扫描电子显微镜(SEM)、傅立叶红外光谱(FT-IR)、X 射线衍射(XRD)和振动样品磁力计(VSM)技术对合成吸附剂的理化性质进行了表征。Fe₃O₄-NH₂@GO的吸附性能与伪秒阶动力学、Elovich和Freundlich等温吸附模型一致,表明其与SFs之间存在各种相互作用,包括π-π相互作用、氢键和静电力。吸附剂对两种具有代表性的 SFs(啶氧菌酯和 E-甲氨基菌酯)的最大吸附量分别为 55.85 mg/g 和 47.35 mg/g。此外,氨基在吸附 SFs 方面表现出显著的潜力。对 MSPE 的参数进行了优化,如吸附剂用量、吸附持续时间、洗脱剂类型和用量以及样品 pH 值。在最佳条件下,所建立的方法在10-2000 µg L-¹范围内表现出令人满意的性能(R² ≥ 0.9969),检出限低(0.01-0.080 µg/kg),分析物回收率高(80.5-104.3 %),精密度好(RSD ≤ 4.96 %,n = 6)。该方法快速、简便、环保、灵敏度高,为开发复杂食品基质中 SFs 的吸附剂提供了新的视角。此外,Fe₃O₄-NH₂@GO 作为一种吸附剂首次用于食品样品中苯基杀菌剂残留的萃取和富集也显示出其广阔的前景,从而为农药残留测定方法的发展做出了贡献。
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来源期刊
Journal of Chromatography A
Journal of Chromatography A 化学-分析化学
CiteScore
7.90
自引率
14.60%
发文量
742
审稿时长
45 days
期刊介绍: The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.
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