Citation: TU Xiang-Ting, YANG Hong-Bo, GUO Feng, ZENG Shi-Yi, TENG Chun-Li, SUN Xiao-Hong, HE Jin-Lin, LIN Shao-Xia. Simultaneous Determination of 16 Kinds of Perfluoroalkyl Substances in Fish Muscle by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2021, 49(4): 528-537. doi: 10.19756/j.issn.0253-3820.211007 shu

Simultaneous Determination of 16 Kinds of Perfluoroalkyl Substances in Fish Muscle by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry

TU Xiang-Ting ^1,2,3 ,
YANG Hong-Bo ^1,3,, ,
GUO Feng ^2,, ,
ZENG Shi-Yi ³ ,
TENG Chun-Li ^1,3 ,
SUN Xiao-Hong ¹ ,
HE Jin-Lin ³ ,
LIN Shao-Xia ³

1.
The Key Laboratory of Environmental Pollution Monitoring and Disease Control, Ministry of Education, School of Public Health, Guizhou Medical University, Guiyang 550025, China;
2.
Key Laboratory of Eco-Geochemistry, Ministry of Natural Resources, National Research Center for Geoanalysis, Beijing 100037, China;
3.
Guizhou Academy of Testing and Analysis, Guiyang 550016, China

Corresponding author: YANG Hong-Bo, GUO Feng,
Received Date: 5 January 2021
Revised Date: 2 March 2021

Fund Project: Supported by the National Natural Science Foundation of China (Nos.21966011, 21976044), the Central Government leading Local Science and Technology Development (No.Qian Ke-Zhong Yin Dit [2016]4001), and the Central Undertakings Basic Research Expenses Special Funds (No.CSJ 201906).

A method for determination of 16 kinds of perfluoroalkyl substances in fish muscle by multi-plug filtration cleanup (m-PFC) combined with ulrahigh performance liquid chromatography-Q-extractive orbitrap high resolution mass spectrometry (UHPLC-Q-Orbitrap HRMS) was established. The samples were ultrasonically extracted by 1% formic acid-acetonitrile, purified by solid phase extraction using m-PFC column and concentrated to 1 mL under nitrogen. The analytes were separated on an Acquity Waters BEH C₁₈ (50 mm×2.1 mm, 1.7 μm) column, and gradient eluted with 5 mmol/L ammonium acetate and methanol. The MS acquisition mode was Full MS/dd-MS² in both negative and positive ionization mode, and the internal standard method was used for quantification. Under the best analytical conditions, a total of 16 target compounds were well separated within 13 min, and the accurate mass deviation of each substance was less than 2.83×10^-6. A good linearity was obtained in the concentration ranges of 0.10-20.0 μg/L with correlation coefficients of greater than 0.990. The MDLs ranged from 0.015 μg/kg to 0.05 μg/kg. The average recoveries of 16 kinds of PFASs spiked at 0.50, 2.0 and 5.0 μg/kg were 70.7%-110.1% and the relative standard deviations (RSDs) were 0.5%-12.8%. The established method was successfully applied to the rapid detection of 25 wild fish samples. Ten PFASs were detected, in which PFOS were the predominant pollutant. The method was simple, rapid, accurate and sensitive, and suitable for the rapid detection of 16 kinds of PFASs in fish muscle.
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