Citation: YANG Xiao, HUANG Huawei, WU Yuan'an, WAN Yiwen, LI Xiaoling, HUANG Xiangrong. Graphene-based pipette tip solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry for determination of ten lipophilic shellfish toxins in shellfish[J]. Chinese Journal of Chromatography, ;2019, 37(5): 505-511. doi: 10.3724/SP.J.1123.2018.11042 shu

Graphene-based pipette tip solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry for determination of ten lipophilic shellfish toxins in shellfish

YANG Xiao ^1,3, ,
HUANG Huawei ^1,3 ,
WU Yuan'an ^1,2 ,
WAN Yiwen ³ ,
LI Xiaoling ³ ,
HUANG Xiangrong ^1,3

1.
Hunan Fisheries Science Institute, Changsha 410153, China;
2.
Collaborative Innovation Center for Efficient and Health Production of Fisheries in Hunan, Changde 415000, China;
3.
Fishery Products Quality Supervision and Testing Center, Ministry of Agriculture, Changsha 410153, China

Received Date: 29 November 2018

Fund Project: Special Fund Project for Quality and Safety Supervision of Agricultural Products (No. 181821301092362)

A method for the simultaneous determination of ten lipophilic shellfish toxins was established based on graphene-based pipette tip solid-phase extraction (G-PT-SPE) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). The factors influencing the extraction efficiency, including the types of extractants, the amount of graphene, the types and volumes of washing and eluent solvents, were optimized in detail. Under the optimal conditions, the calibration curves showed linear relationships between the LC peak areas of the selected ion-pairs and the mass concentrations of the ten lipophilic shellfish toxins with correlation coefficients >0.99. The limits of detection (LODs) and the limits of quantification (LOQs) of the method were 0.1-1.1 μg/kg and 0.3-3.2 μg/kg, respectively. The recoveries of the ten lipophilic shellfish toxins spiked in blank oyster at three levels ranged from 72.0% to 101.2% with relative standard deviations <15%. The method is sensitive, simple, and effective, and is suitable for the determination of the lipophilic shellfish toxins in shellfish products.
- graphene,
- pipette tip solid-phase extraction,
- liquid chromatography-tandem mass spectrometry (LC-MS/MS),
- lipophilic shellfish toxins,
- shellfish
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