Citation: SONG Wei, ZHOU Dian-Bing, GUO Chun-Li, HAN Fang, DING Lei, LYU Ya-Ning, JIA Xue-Ying, ZHENG Ping, DENG Xiao-Jun. Determination of Multiresidue of Pesticide in Chrysanthemum by Magnetic Fullerene Dispersive Solid Phase Extraction with Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2021, 49(9): 1587-1596. doi: 10.19756/j.issn.0253-3820.191683 shu

Determination of Multiresidue of Pesticide in Chrysanthemum by Magnetic Fullerene Dispersive Solid Phase Extraction with Liquid Chromatography-Tandem Mass Spectrometry

SONG Wei ^1,2,, ,
ZHOU Dian-Bing ^1,2 ,
GUO Chun-Li ¹ ,
HAN Fang ^1,2 ,
DING Lei ^1,2 ,
LYU Ya-Ning ^1,2 ,
JIA Xue-Ying ¹ ,
ZHENG Ping ^1,2 ,
DENG Xiao-Jun ³

1.
Technical Center for Hefei Customs, Hefei 230022, China;
2.
Anhui Province Key Laboratory of Analysis and Detection for Food Safety, Hefei 230022, China;
3.
Animal, Plant and Food Inspection & Quarantine Center, Shanghai Customs, Shanghai 200135, China

Corresponding author: SONG Wei, songwei1768@163.com
Received Date: 18 November 2019
Revised Date: 19 May 2021

Fund Project: Supported by the Research Projects of the General Administration of Customs, China (No.2017IK108), the External Cooperation Program of Anhui Province, China (No.1804b06020349) and the Research Projects of Shanghai Science Committee, China (No.19395810100).

Magnetic fullerene (Fe₃O₄@SiO₂@C₆₀) was synthesized as a solid-phase extraction adsorbent for extraction and enrichment of pesticides in Chrysanthemum. Based on this, anultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was developed for determination of nine kinds of pesticides, including cyprodinil, zoxamide, tolfenpyrad, azoxystrobin, pyraclostrobin, trifloxystrobin, fenpyroximate, pyridaben and phoxim in edible chrysanthemum. The results showed that the Fe₃O₄@SiO₂@C₆₀ had obvious adsorption to cyprodinil, zoxamide, tolfenpyrad, azoxystrobin, pyraclostrobin, trifloxystrobin, fenpyroximate, pyridaben and phoxim. The influence factors of magnetic dispersion solid phase extraction were investigated, and it was found that a best extraction was obtained under the optimal conditions such as 30.0 mg of Fe₃O₄@SiO₂@C₆₀ as adsorbent, extraction for 20 min under shaking, separation of the Fe₃O₄@SiO₂@C₆₀ by an external magnetic field, and elution two times with 1 mL of ethyl acetate. The result showed that Fe₃O₄@SiO₂@C₆₀ had good stability and reusability. All of the tested pesticides showed good linear relationship in the range of concentration 0.005-0.1 mg/L with correlation coefficients of greater than 0.999. The detection limits and the quantitation limits of nine target pesticides were in the range of 0.001-0.003 mg/kg and 0.003-0.01 mg/kg, respectively. When the addition levels of the pesticides were 0.01, 0.05 and 0.10 mg/kg, the recoveries of the method ranged from 71.0% to 94.6% with the relative standard deviations (n=6) ranging from 4.6% to 11.3%. The method was simple, sensitive, fast and with low cost, and suitable for the accurate qualitative and quantitative determination of nine pesticides in chrysanthemum.
- Magnetic fullerene,
- Dispersive solid phase extraction,
- Liquid chromatography-tandem mass spectrometry,
- Pesticide residues,
- Chrysanthemum
1. [1]
2. [2]
3. [3]
  QIN J A, FU Y W, LU Q, DOU X W, LUO J Y, YANG M H. Microchem. J., 2021, 160:105681-105689.
4. [4]
5. [5]
6. [6]
7. [7]
8. [8]
  EU Pesticides Database (2021). https://ec.europa.eu/food/plant/pesticides/eu-pesticides-database/mrls/?event=download.MRL.
9. [9]
10. [10]
11. [11]
12. [12]
13. [13]
  SHI Z H, HU J D, LI Q, ZHANG S L, LIANG Y H, ZHANG H Y. J. Chromatogr. A, 2014, 1355:219-277.
14. [14]
  HAN Q, WANG Z H, XIA J F, ZHANG X Q, WANG H W, DING M Y.J. Sep. Sci., 2014, 37(1-2):99-105.
15. [15]
  DENG X J, GUO Q J, CHEN X P, XUE T, WANG H, YAO P. Food Chem., 2014, 145(15):853-858.
16. [16]
17. [17]
18. [18]
  LI X S, ZHU G T, LUO Y B, YUAN B F, FENG Y Q. TrAC-Trends Anal. Chem., 2013, 45:234-247.
19. [19]
  DU Z, LIU M, LI G K. J. Sep.Sci., 2013, 36(20):3387-3394.
20. [20]
21. [21]
  ZHANG Y, ZHOU H, ZHANG Z H, WU X L, CHENW G, ZHU Y, FANG C F, ZHAOY G. J. Chromatogr. A, 2017, 1489:29-38.
22. [22]
  LIU G Y, LI L Y, HUANG X D, ZHENG S N, XU X M, LIU Z X, ZHANG Y G, WANG J, LIN H, XU D H. J. Mater.Sci., 2018, 53(15):10772-10783.
23. [23]
  WU J R, ZHAO H Y, XIAO D L, CHUONG P H, HE J, HE H. J. Chromatogr. A, 2016, 1454:1-8.
24. [24]
25. [25]
  GAN N, ZHANG J B, LIN S C, LONG N B, LI T H, CAO Y T. Materials, 2014, 7(8):6028-6044.
26. [26]
  WANG W N, MA R Y, WU Q H, WANG C, WANG Z. J.Chromatogr. A, 2013, 1293:20-27.
27. [27]
  ZHOU D B, SHENGX, HAN F, HU Y Y, DING L, LV Y N, SONG W, ZHENG P. J. Chromatogr. A, 2018, 1578:53-60.
28. [28]
  SERRANO A, GALLEGO M. J. Sep.Sci., 2006, 29(1):33-40.
29. [29]
  GOSETTI F, MAZZUCCO E, ZAMPIERI D, GENNARO M C. J. Chromatogr. A, 2010, 1217:3929-3937.
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