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Citation: GUO Meng-Meng, GUO Jiao, WU Hai-Yan, TAN Zhi-Jun, ZHAI Yu-Xiu, WANG Zhi, LI Zhao-Xin, LI Feng-Ling. Rapid Screening and Confirmation of Perfluorinated Compounds and Their Precursors in Fish Muscle by Solid Phase Extraction Purification and Liquid Chromatography Coupled with Quadrupole/Exactive Orbitrap Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2016, 44(10): 1504-1513. doi: 10.11895/j.issn.0253-3820.160333 shu

Rapid Screening and Confirmation of Perfluorinated Compounds and Their Precursors in Fish Muscle by Solid Phase Extraction Purification and Liquid Chromatography Coupled with Quadrupole/Exactive Orbitrap Mass Spectrometry

1.
Key Laboratory of Testing and Evaluation for Aquatic Product Safety and Quality, Ministry of Agriculture, P. R. China; Yellow Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Qingdao 266071, China;
2.
Ocean University of China, Qingdao 266100, China;
3.
Qingdao Institute of Product Quality Inspection and Technical Research, Qingdao Product Quality Supervision and Testing Research, Qingdao 266061, China

Received Date: 26 April 2016
Revised Date: 17 June 2016

Fund Project: This work was supported by the National Science and Technology Basic Work (No.2014FY230100)

Figures(3)

A method was developed for the rapid screening and confirmation of 18 perfluorinated compounds (PFCs) and 21 precursors in fish muscle by solid phase extraction and liquid chromatography coupled with quadrupole/exactive orbitrap mass spectrometry (LC-Q Exactive Orbitrap MS). In this method, the sample was firstly extracted with acetonitrile-water (90:10, V/V), cleaned-up by solid-phase extraction using Oasis PRiME HLB column. Then, 39 target compounds were separated on a BEH C₁₈ (2.1 mm×100 mm, 1.7 μm) column, and the background interference caused by LC system was eliminated by a short C₁₈ HPLC column located between the mixer and the auto sampler. In the process of quantification and qualification, a full MS/dd-MS² experiment was adopted in mass spectrometry acquisition, accompanied with the full scan MS date for quantification, as well as the date dependent MS² product ion spectra for qualification. The mass accuracy error was less than 3×10^-6, and the calibration curves were linear well with correlation coefficient over 0.99. The limits of detection ranged from 0.02 to 0.50 μg/kg. The average spiked recoveries for 39 target compounds were between 61.7% and 122.0%, with relative standard derivations (RSDs) from 6.9% to 18.8%. The developed method was successfully applied to the simultaneous determination of 18 PFCs and 21 precursors in fish muscle with satisfactory results.
- Perfluorinated compounds and their precursors,
- Fish muscle,
- Quadrupole/exactive orbitrap mass spectrometry,
- Solid phase extraction
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