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引用本文:   黄斯敏, 胡玉斐, 陈彦龙, 李攻科, 夏凌. 磁性共价有机骨架固相萃取-高效液相色谱测定柑橘中农药残留. 分析化学, 2020, 48(10): 1392-1399. doi:  10.19756/j.issn.0253-3820.201359 [复制]

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 [复制]

磁性共价有机骨架固相萃取-高效液相色谱测定柑橘中农药残留

通讯作者:  李攻科, cesgkl@mail.sysu.edu.cn; 夏凌, xialing@mail.sysu.edu.cn

收稿日期: 2020-06-19

基金项目: 本文系广东省重点领域研发计划项目(No.2019B020211001)、国家自然科学基金项目(Nos.21675178,21976213,21804147)、国家重点研发计划项目(No.2019YFC1606101)和广东省自然科学基金项目(No.2018A030313241)资助

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).

制备了具有核壳结构的磁性共价有机骨架复合材料(Fe3O4@COF),并将其作为磁性固相萃取的吸附剂,结合高效液相色谱-紫外检测器法(HPLC-UV),建立了测定柑橘类水果中噻虫嗪、吡虫啉、多菌灵和噻菌灵等农药残留的分析方法。通过扫描电子显微镜、透射电子显微镜、傅里叶变换红外光谱、X射线粉末衍射和磁学性能测试对材料进行了表征。考察了磁性固相萃取的影响因素,得到最佳的萃取条件:将20.0 mg Fe3O4@COF分散于10 mL柑橘类水果样品溶液中,振荡20 min,磁性分离,用1 mL甲醇振荡5 min后洗脱,洗脱液待HPLC-UV分析。噻虫嗪、多菌灵和噻菌灵在1~1000 μg/L浓度范围内、吡虫啉在5-1000 μg/L浓度范围内与色谱峰面积具有良好的线性关系,检出限为0.27~1.22 μg/L,加标回收率为92.1%~104.0%,RSD为1.2%~8.3%。本方法操作简单,检出限低,线性范围宽,适用于柑橘类样品中的4种农药残留的同时分析。

关键词:   磁性固相萃取, 高效液相色谱, 农药残留, 柑橘类水果
Key words:   Magnetic solid-phase extraction, High performance-liquid chromatography, Pesticide residue, Citrus
[1]

Prabhaker N, Castle S J, Naranjo S E, Toscano N C, Morse J G. J. Econ. Entomol., 2011, 104(3):773-781

[2]

Wang P, Yang X, Wang J, Cui J, Dong A J, Zhao H T, Zhang L W, Wang Z Y, Xu R B, Li W J, Zhang Y C, Zhang H, Jing J. Food Chem., 2012, 134(3):1691-1698

[3]

Campillo N, Viñas P, Férez-Melgarejo G, Hernández-Córdoba M. J. Agric. Food Chem., 2013, 61(20):4799-4805

[4]

Xia L, Yang J N, Su R H, Zhou W J, Zhang Y S, Zhong Y H, Huang S M, Chen Y L, Li G K. Anal. Chem., 2020, 92(1):34-48

[5]

Jiang H L, Li N, Cui L, Wang X, Zhao R S. TrAC-Trends Anal. Chem., 2019, 120:115632

[6]

Maya F, Cabello C P, Frizzarin R M, Estela J M, Palomino G T, Cerdà V. TrAC-Trends Anal. Chem., 2017, 90:142-152

[7]

Wierucka M, Biziuk M. TrAC-Trends Anal. Chem., 2014, 59:50-58

[8]

Ding S Y, Wang W. Chem. Soc. Rev., 2013, 42(2):548-568

[9]

Huang N, Chen X, Krishna R, Jiang D L. Angew. Chem. Int. Ed., 2015, 54(10):2986-2990

[10]

Zeng Y F, Zou R Q, Zhao Y L. Adv. Mater., 2016, 28(15):2855-2873

[11]

Fang Q R, Gu S, Zheng J, Zhuang Z B, Qiu S L, Yan Y S. Angew. Chem. Int. Ed., 2014, 53(11):2878-2882

[12]

Xu H, Gao J, Jiang D L. Nat. Chem., 2015, 7(11):905-912

[13]

Ding X S, Guo J, Feng X, Honsho Y, Guo J D, Seki S, Maitarad P, Saeki A, Nagase S, Jiang D L. Angew. Chem. Int. Ed., 2011, 50(6):1289-1293

[14]

Dogru M, Handloser M, Auras F, Kunz T, Medina D, Hartschuh A, Knochel P, Bein T. Angew. Chem. Int. Ed., 2013, 52(10):2920-2924

[15]

Li Z P, Zhang Y W, Xia H, Mu Y, Liu X M. Chem. Commun., 2016, 52(39):6613-6616

[16]

Sun Q, Aguila B, Earl L D, Abney C W, Wojtas L, Thallapally P K, Ma S Q. Adv. Mater., 2018, 30(20):1705479

[17]

Wu M X, Chen G, Liu P, Zhou W H, Jia Q. J. Chromatogr. A, 2016, 1456:34-41

[18]

Ji W H, Guo Y S, Wang X, Lu X F, Guo D S. J. Chromatogr. A, 2019, 1595:11-18

[19]

Deng H, Li X L, Peng Q, Wang X, Chen J P, Li Y D. Angew. Chem. Int. Ed., 2005, 44(18):2782-2785

[20]

Huang Y F, Li Y, Jiang Y, Yan X P. J. Anal. At. Spectrom., 2010, 25(9):1467-1474

[21]

Dong J Q, Wang Y X, Liu G L, Cheng Y D, Zhao D. Crystengcomm, 2017, 19(33):4899-4904

[22]

Frisch M J, Trucks G W, Schlegel H B, Cuseria S G E, Robb M A, Cheeseman J R, Scalmani G, Barone V, Mennucci B, Petersson G A, Nakatsuji H, Caricato M, Li X, Hratchian H P, Izmaylov A F, Bloino J, Zheng G, Sonnenberg J L, Hada M, Ehara M, Toyota K, Fukuda R, Hasegawa J, Ishida M, Nakajima T, Honda Y, Kitao O, Nakai H, Vreven T, Montgomery J A J, Peralta J E, Ogliaro F, Bearpark M, Heyd J J, Brothers E, Kudin K N, Staroverov V N, Kobayashi R, Normand J, Raghavachari K, Rendell A, Burant J C, Iyengar S S, Tomasi J, Cossi M, Rega N, Millam N J, Klene M, Knox J E, Cross J B, Bakken V, Adamo C, Jaramillo J, Gomperts R, Stratmann R E, Yazyev O, Austin A J, Cammi R, Pomelli C, Ochterski J W, Martin R L, Morokuma K, Zakrzewski V G, Voth G A, Salvador P, Dannenberg J J, Dapprich S, Daniels A D, Farkas O, Foresman J B, Ortiz J V, Cioslowski J, Fox D J. Gaussian Inc., Wallingford CT, 2009

[23]

Liu L, Hao Y H, Zhou X, Wang C, Wu Q H, Wang Z. Anal. Methods, 2015, 7(6):2762-2769

[24]

Díaz-Álvarez M, Turiel E, Martín-Esteban A. Anal. Chim. Acta, 2019, 1045:117-122

[25]

Liang G H, Guo X J, Tan X C, Mai S F, Chen Z G, Zhai H Y. Microchem. J., 2019, 146:1285-1294

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磁性共价有机骨架固相萃取-高效液相色谱测定柑橘中农药残留

黄斯敏, 胡玉斐, 陈彦龙, 李攻科, 夏凌

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