Citation: HUANG Si-Min, HU Yu-Fei, CHEN Yan-Long, LI Gong-Ke, XIA Ling. Magnetic Solid-phase Extraction Coupled with High-Performance Liquid Chromatography for Pesticide Residues Analysis in Citrus Sample[J]. Chinese Journal of Analytical Chemistry, ;2020, 48(10): 1392-1399. doi: 10.19756/j.issn.0253-3820.201359 shu

Magnetic Solid-phase Extraction Coupled with High-Performance Liquid Chromatography for Pesticide Residues Analysis in Citrus Sample

School of Chemistry, Sun Yat-sen University, Guangzhou 510275, China

Received Date: 19 June 2020
Revised Date: 4 August 2020

Fund Project: This work was supported by the Research and Development Plan for Key Areas of Food Safety in Guangdong Province of China (No. 2019B020211001), the National Natural Science Foundation of China (Nos. 21675178, 21976213, 21804147), the National Key Research and Development Program of China (No. 2019YFC1606101) and the Guangdong Provincial Natural Science Foundation of China (No.2018A030313241).

The Fe₃O₄@COF with core-shell structures was synthesized and used as sorbent in magnetic solid-phase extraction (MSPE). This Fe₃O₄@COF-MSPE method coupled with high-performance liquid chromatography-ultraviolet detector (HPLC-UV) was employed for simultaneous analysis of thiamethoxam, imidacloprid, carbendazim and thiabendazole residues in citrus samples. The synthesized Fe₃O₄@COF was characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectra, X-ray diffraction and magnetometry techniques. The operation conditions of MSPE were optimized. In each trial, 20.0 mg of Fe₃O₄@COF was dispersed into 10 mL of citrus sample and shaken for 20 min. Then, the Fe₃O₄@COF was separated by an external magnetic field. Next, the pesticide target compounds were eluted from Fe₃O₄@COF with 1 mL of methanol and shaken for 5 min. Under the optimized conditions, the method had an excellent linearity in the concentration range of 1-1000 μg/L for thiomethoxam, carbendazim and thiabendazle, and 5-1000 μg/L for imidacloprid. The limits of detection ranged from 0.27 μg/L to 1.22 μg/L. The recoveries ranged from 92.1% to 104.0%. The relative standard deviations (RSDs) ranged from 1.2% to 8.3%. The proposed Fe₃O₄@COF-MSPE-HPLC-UV method was demonstrated to be easy operation, low limit of detection and wide detection range, which was applicable to simultaneous determination of four pesticide residues in citrus samples.
- Magnetic solid-phase extraction,
- High performance-liquid chromatography,
- Pesticide residue,
- Citrus
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