Citation: SUN Xiao-Jie, DING Hai-Yan, TAN Jie, XING Jun, . Research on Octyl-functionalized Ionic Liquid Bonding Silica Gel for Solid Phase Extraction of Shellfish Toxins in Seawater[J]. Chinese Journal of Analytical Chemistry, ;2020, 48(1): 104-112. doi: 10.19756/j.issn.0253-3820.191367 shu

Research on Octyl-functionalized Ionic Liquid Bonding Silica Gel for Solid Phase Extraction of Shellfish Toxins in Seawater

SUN Xiao-Jie ^1, ,
DING Hai-Yan ¹ ,
TAN Jie ^1,2 ,
XING Jun ³ ,
¹ ,
¹ ,
¹ ,
¹

1.
Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality, Ministry of Agriculture and Rural Affairs;Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Qingdao 266071, China;
2.
Qingdao National Laboratory for Marine Science and Technology, Qingdao 266000, China;
3.
Key Laboratory of Analytical Chemistry for Biology and Medicine(Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China

Received Date: 27 June 2019
Revised Date: 7 November 2019

Fund Project: This work was supported by the National Key R&D Program of China (No. 2017YFC1600705), the Special Scientific Research Funds for Central Non-profit Institutes, Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences (Nos. 20603022016007, 20603022017015) and the National Natural Science Foundation of China (No. 21207162).

Shellfish toxins are a kind of important marine pollutant. In this study, a novel ionic liquid bonded silica gel material (silica-[SOIM] [PF₆]) was prepared by grafting octyl-functionalized ionic liquid onto silica gel, which was characterized and analyzed by infrared spectroscopy (IR), nuclear magnetic resonance (NMR), and elemental analysis. Solid phase extraction cartridge of silica-[SOIM] [PF₆], coupled with LC-MS/MS technique was used to extract and determine the concentration of shellfish toxins[Okadaic acid (OA), Dinophysistoxin-1 (DTX-1) and Dinophysistoxin-2 (DTX-2)] in seawater for the first time. It was found that the solid phase extraction material silica-[SOIM] [PF₆] had multiple interactions with the 3 kinds of shellfish toxins, such as hydrophobic and ion-exchange. The method was optimized in aspects of volume and pH of the loaded sample solution, as well as the usage of rinsing and eluting reagents. Results indicated that the silica-[SOIM] [PF₆] had good extraction effect on target shellfish toxins in seawater, which was better than or equivalent to the performance of commercial extraction materials. The method had a good linearity (R²>0.995) in the concentration range of shellfish toxins from 0.02 μg/L to 2.50 μg/L, with limit of detection (LOD) of 0.01 μg/L and limit of quantification (LOQ) of 0.05 μg/L. The average recoveries for 3 kinds of shellfish toxins were 93.0%-116.0% at different spiking levels in blank seawater. Simultaneously, the material had good reproducibility, with the relative standard deviation (RSD) of less than 15% intra-and inter-batch. This method was accurate, sensitive, simple and reliable, and could be used for the extraction and detection of shellfish toxins in actual samples.
- Ionic liquid,
- Solid phase extraction,
- Multiple mode,
- Shellfish toxins,
- Seawater
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