Determination of Fungicides in Fresh Fruit Juice Using Magnetic Solid-Phase Extraction Coupled With Gas Chromatography-Triple Quadrupole Mass Spectrometry.

IF 1.5 4区 化学 Q4 BIOCHEMICAL RESEARCH METHODS
Qinghua Yang, Honghai Deng, Yilan Shi, Qianying Qiu, Jinxin Wang, Wenhui Ping, Jun Gu, Weibing Zhang
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Abstract

A fast, simple and effective method was developed and validated for determination of 11 fungicides using magnetic solid-phase extraction with NH2-Fe3O4@GO (graphene oxide) combined with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). To carry out the extraction of the fungicides from samples, NH2-Fe3O4@GO nanocomposites were synthesized and characterized by scanning electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. The target analytes were extracted on NH2-Fe3O4@GO and then eluted by ethyl acetate and acetonitrile (1:1 v/v). Finally, the extraction solvent concentrated by nitrogen blowing was analyzed by GC-MS/MS, which demonstrated good linearity between 0.05 and 5.0 mg L-1. The limits of detection (signal-to-noise ratio = 3) and the limits of quantification (signal-to-noise ratio = 10) for the 11 fungicides ranged from 1.0 to 3.5 and 3.0 to 10.5 μg kg-1, respectively. The accuracy and precision of the proposed method were evaluated by measuring tagged samples; the recoveries and relative standard deviations ranged from 75.3% to 103.9% and 2.19% to 4.68%, respectively. The utility of the adsorbent was demonstrated to determine trace fungicides in fresh fruit juice samples.

磁固相萃取-气相色谱-三重四极杆质谱联用测定鲜榨果汁中的杀菌剂。
建立了NH2-Fe3O4@GO(氧化石墨烯)磁固相萃取联合气相色谱-三重四极杆质谱(GC-MS/MS)测定11种杀菌剂的快速、简便、有效方法,并进行了验证。为了从样品中提取杀菌剂,合成了NH2-Fe3O4@GO纳米复合材料,并通过扫描电镜、傅里叶变换红外光谱和x射线衍射对其进行了表征。在NH2-Fe3O4@GO上提取目标物,然后用乙酸乙酯和乙腈(1:1 v/v)洗脱。最后,采用气相色谱-质谱联用技术对氮吹浓缩提取溶剂进行分析,结果表明,提取溶剂在0.05 ~ 5.0 mg L-1之间呈良好的线性关系。11种杀菌剂的检出限(信噪比为3)和定量限(信噪比为10)分别为1.0 ~ 3.5和3.0 ~ 10.5 μg kg-1。通过对标记样品的测量,评估了该方法的准确性和精密度;加样回收率为75.3% ~ 103.9%,相对标准偏差为2.19% ~ 4.68%。用该吸附剂测定鲜榨果汁中痕量杀菌剂。
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来源期刊
CiteScore
2.90
自引率
7.70%
发文量
94
审稿时长
5.6 months
期刊介绍: The Journal of Chromatographic Science is devoted to the dissemination of information concerning all methods of chromatographic analysis. The standard manuscript is a description of recent original research that covers any or all phases of a specific separation problem, principle, or method. Manuscripts which have a high degree of novelty and fundamental significance to the field of separation science are particularly encouraged. It is expected the authors will clearly state in the Introduction how their method compares in some markedly new and improved way to previous published related methods. Analytical performance characteristics of new methods including sensitivity, tested limits of detection or quantification, accuracy, precision, and specificity should be provided. Manuscripts which describe a straightforward extension of a known analytical method or an application to a previously analyzed and/or uncomplicated sample matrix will not normally be reviewed favorably. Manuscripts in which mass spectrometry is the dominant analytical method and chromatography is of marked secondary importance may be declined.
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