基于磁性共轭微孔聚合物的超高效液相色谱-串联质谱法测定果蔬中7种有机磷杀虫剂

引用本文: 蔡伟秋, 雷皓宇, 胡玉玲, 李攻科. 基于磁性共轭微孔聚合物的超高效液相色谱-串联质谱法测定果蔬中7种有机磷杀虫剂[J]. 色谱, 2020, 38(1): 113-119. doi: 10.3724/SP.J.1123.2019.06033 shu

Citation: CAI Weiqiu, LEI Haoyu, HU Yuling, LI Gongke. Determination of seven organophosphorus insecticides in fruits and vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry based on magnetic conjugated microporous polymers[J]. Chinese Journal of Chromatography, 2020, 38(1): 113-119. doi: 10.3724/SP.J.1123.2019.06033 shu

基于磁性共轭微孔聚合物的超高效液相色谱-串联质谱法测定果蔬中7种有机磷杀虫剂

中山大学化学学院, 广东广州 510275

通讯作者: 胡玉玲,E-mail:ceshyl@mail.sysu.edu.cn; 李攻科,E-mail:cesgkl@mail.sysu.edu.cn

基金项目:
广州市科技计划项目（201704020040）；国家自然科学基金（21575168）；广东省自然科学基金（2017A030313070）；广东省食品安全重点领域研发计划（2019B020211001）.

摘要: 建立了基于磁性共轭微孔聚合物的磁固相萃取-超高效液相色谱-串联质谱（UPLC-MS/MS）测定果蔬中7种有机磷杀虫剂的方法。将亚苯基亚乙炔基修饰的Fe₃O₄与1，3，5-三溴苯、1，3，5-三乙炔苯反应，制备磁性共轭微孔聚合物，材料能有效吸附共轭结构的有机磷杀虫剂，并在外磁场中实现便捷磁分离。方法的检出限（LOD）为0.12~5.0 ng/kg，加标回收率为80.8%~125%，相对标准偏差（RSD）小于6%（n=5）。方法应用于分析市场上果蔬样品中7种有机磷杀虫剂，检出含量为1.1~500.0 ng/kg。该方法灵敏度高，准确可靠，对果蔬中有机磷杀虫剂的检测具有良好的应用潜力。

关键词:

English

Determination of seven organophosphorus insecticides in fruits and vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry based on magnetic conjugated microporous polymers

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

Corresponding author: HU Yuling, ; LI Gongke,

Received Date: 29 June 2019
Fund Project:
Guangzhou Science and Technology Program of China (No. 201704020040)

Abstract: A method was developed for the determination of seven organophosphorus insecticides in fruits and vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) based on magnetic conjugated microporous polymers (CMPs). Fe₃O₄ nanoparticles modified by phenylene and ethynylene were cross-linked with 1,3,5-tribromobenzene and 1,3,5-trialkynylbenzene to obtain magnetic CMPs. This material with a three-dimensional network structure and covalently built-in Fe₃O₄ nanoparticles could effectively enrich organophosphorus insecticides with a conjugated structure, thus allowing for convenient magnetic separation in an external magnetic field. Under the optimized conditions, the seven organophosphorus pesticides were extracted by using the magnetic CMPs as magnetic solid phase extraction adsorbents. The limits of detection (LODs) of the seven target analytes were in the range of 0.12-5.0 ng/kg. The recoveries were between 80.8% and 125%, and the relative standard deviations (RSDs, n=5) were less than 6%. The organophosphorus insecticides were detected in fruits and vegetables at concentrations in the range of 1.1-500.0 ng/kg. The method is sensitive, accurate and reliable, and it shows good application potential for the determination of the organophosphorus pesticides in fruits and vegetables.

Key words:

1. [1] Liu J, Lu W H, Cui R, et al. Chinese Journal of Chromatography, 2018, 36(1):30 刘洁, 鹿文慧, 崔荣, 等. 色谱, 2018, 36(1):30
2. [2] Li M H, Jiao C N, Yang X M, et al. Anal Methods, 2017, 9(4):593
3. [3] Farajzadeh M A, Bamorowat M, Mogaddam M R A. RSC Adv, 2016, 6(114):112939
4. [4] GB 2763-2016
5. [5] Nadereh R, Elnaz B, Zahra R. Food Anal Method, 2017, 10(7):2229
6. [6] Neha S, Supriya K, Kishore N. J AOAC Int, 2017, 100(3):804
7. [7] Huang T T, Tang Y, Dong X Q. Food Science, 2018, 39(6):315 黄田田, 汤桦, 董晓倩, 等. 食品科学, 2018, 39(6):315
8. [8] Song X J, He X R, Yin M M, et al. Chinese Journal of Chromatography, 2018, 36(10):1038 宋晓娟, 贺心然, 尹明明, 等. 色谱, 2018, 36(10):1038
9. [9] Wang L Z, Zhou Y, Chen Y, et al. Chinese Journal of Chromatography, 2012, 30(2):146 王连珠, 周昱, 陈泳, 等. 色谱, 2012, 30(2):146
10. [10] Khalifa M E, Kenawy I M M, Abou E Y G. J Environ Chem Eng, 2017, 5(4):3447
11. [11] Zuo H G, Zhu J X, Zhan C R, et al. Environ Monit Assess, 2015, 187(394):1
12. [12] Wang Y L, Gao Y L, Wang P P. Talanta, 2013, 115:920
13. [13] Ma J K, Huang X C, Wei S L. J Sep Sci, 2018, 41:3152
14. [14] Hasan B, Hatam A, Yadollah Y, et al. Microchim Acta, 2018, 185(62):1
15. [15] Shokouh M, Hassan S, Majid B. J Chromatogr A, 2015, 1406:48
16. [16] Zahra A, Raana J. Chromatographia, 2017, 80(9):1411
17. [17] Zahra A, Raana J, Amir A M. Anal Method, 2017, 9(31):4547
18. [18] Zhou L J, Hu Y L, Li G K. Anal Chem, 2016, 88(13):6930
19. [19] Li G, Liu Q Q, Liao B, et al. Eur Polym J, 2017, 93:556
20. [20] Lei H Y, Hu Y L, Li G K. J Chromatogr A, 2018, 1580(14):22
21. [21] Dawood K M, Hassaneen H M, Abdelhadi H A, et al. J Braz Chem Soc, 2014, 25(9):1688
22. [22] Liang D Q, Su K M, Zhang J M, et al. Food Science, 2014, 35(4):159 梁达清, 苏肯明, 张菊梅, 等. 食品科学, 2014, 35(4):159

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基于磁性共轭微孔聚合物的超高效液相色谱-串联质谱法测定果蔬中7种有机磷杀虫剂

通讯作者: 胡玉玲,E-mail:ceshyl@mail.sysu.edu.cn; 李攻科,E-mail:cesgkl@mail.sysu.edu.cn

English

Determination of seven organophosphorus insecticides in fruits and vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry based on magnetic conjugated microporous polymers

Corresponding author: HU Yuling, ; LI Gongke,

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

基于磁性共轭微孔聚合物的超高效液相色谱-串联质谱法测定果蔬中7种有机磷杀虫剂

通讯作者: 胡玉玲,E-mail:ceshyl@mail.sysu.edu.cn; 李攻科,E-mail:cesgkl@mail.sysu.edu.cn

English

Determination of seven organophosphorus insecticides in fruits and vegetables by ultra-high performance liquid chromatography-tandem mass spectrometry based on magnetic conjugated microporous polymers

Corresponding author: HU Yuling, ; LI Gongke,

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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