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            引用本文:   黃斯敏, 胡玉斐, 陳彥龍, 李攻科, 夏凌. 磁性共價有機骨架固相萃取-高效液相色譜測定柑橘中農藥殘留. 分析化學, 2020, 48(10): 1392-1399. doi:  10.19756/j.issn.0253-3820.201359 [復制]

            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. Chinese Journal of Analytical Chemistry, 2020, 48(10): 1392-1399. doi: 10.19756/j.issn.0253-3820.201359 [復制]

            磁性共價有機骨架固相萃取-高效液相色譜測定柑橘中農藥殘留

            通訊作者:  李攻科, cesgkl@mail.sysu.edu.cn; 夏凌, xialing@mail.sysu.edu.cn

            收稿日期: 2020-06-19

            基金項目: 本文系廣東省重點領域研發計劃項目(No.2019B020211001)、國家自然科學基金項目(Nos.21675178,21976213,21804147)、國家重點研發計劃項目(No.2019YFC1606101)和廣東省自然科學基金項目(No.2018A030313241)資助

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

            Corresponding author:  LI Gong-Ke , cesgkl@mail.sysu.edu.cn; XIA Ling , xialing@mail.sysu.edu.cn

            Received Date:  2020-06-19

            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).

            制備了具有核殼結構的磁性共價有機骨架復合材料(Fe3O4@COF),并將其作為磁性固相萃取的吸附劑,結合高效液相色譜-紫外檢測器法(HPLC-UV),建立了測定柑橘類水果中噻蟲嗪、吡蟲啉、多菌靈和噻菌靈等農藥殘留的分析方法。通過掃描電子顯微鏡、透射電子顯微鏡、傅里葉變換紅外光譜、X射線粉末衍射和磁學性能測試對材料進行了表征??疾炝舜判怨滔噍腿〉挠绊懸蛩?,得到最佳的萃取條件:將20.0 mg Fe3O4@COF分散于10 mL柑橘類水果樣品溶液中,振蕩20 min,磁性分離,用1 mL甲醇振蕩5 min后洗脫,洗脫液待HPLC-UV分析。噻蟲嗪、多菌靈和噻菌靈在1~1000 μg/L濃度范圍內、吡蟲啉在5-1000 μg/L濃度范圍內與色譜峰面積具有良好的線性關系,檢出限為0.27~1.22 μg/L,加標回收率為92.1%~104.0%,RSD為1.2%~8.3%。本方法操作簡單,檢出限低,線性范圍寬,適用于柑橘類樣品中的4種農藥殘留的同時分析。

            關鍵詞:   磁性固相萃取, 高效液相色譜, 農藥殘留, 柑橘類水果
            Key words:   Magnetic solid-phase extraction, High performance-liquid chromatography, Pesticide residue, Citrus
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            目錄

            磁性共價有機骨架固相萃取-高效液相色譜測定柑橘中農藥殘留

            黃斯敏, 胡玉斐, 陳彥龍, 李攻科, 夏凌

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