Page 37 - 理化检验-化学分册2025年第三期

邹 淼，等：超高效液相色谱-串联质谱法同时测定鱼肉中23种全氟和多氟烷基物质的含量

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Simultaneous Determination of 23 Perfluorinated and Polyfluoroalkyl
Substances in Fish by Ultra-High Performance Liquid

Chromatography-Tandem Mass Spectrometry

ZOU Miao, FENG Jing, HAN Xiaoou, HUA Zhenggang *

(Center for Disease Control and Prevention of Liaoning Province, Shenyang 110005, China)
Abstract: The current determination methods of perfluorinated and polyfluoroalkyl substances (PFASs) did not involve the
new PFASs, and were difficult to meet the requirements of simultaneous determination of PFASs, especially the low recoveries
of long-chain compounds. In order to solve the above problems, the method mentioned by the title was proposed. The fish
sample (2.000 g) was taken and mixed well with 20 μL of 100 μg · L 13 PFASs mixed isotopic internal standard solution and
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2.0 mL of water, and then 10.0 mL of acetonitrile solution containing 1%(volume fraction) formic acid was added. The mixture
was vortex oscillated for 30 min, and centrifuged for 10 min. The supernatant was taken and purified by pass-through Anavo
HMR-Lipid solid phase extraction column. The purified solution obtained was blown to dryness by nitrogen at 40 ℃. The residue
was redissolved with 0.4 mL of methanol. After swirl mixing and centrifugation for 5 min, the supernatant was taken, in which
23 PFASs [ including 2 new PFASs of 6∶2 chloropolyfluoroalkyl ether sulfonate (6/2F-53B) and 8∶2 chloropolyfluoroalkyl
ether sulfonate (8/2F-53B)] were simultaneously determined by ultra-high performance liquid chromatography-tandem mass
spectrometry (UHPLC-MS/MS) using Acquity UPLC BEH C column as the stationary phase, and a mixture of methanol and
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2 mmol · L ammonium formate solution at different volume ratios as the mobile phase for gradient elution. In mass spectrometry
analysis, the negative ion mode of the electrospray ion source was used for scanning. The isotope internal standard method was
used for quantification. As shown by the results, the linear ranges of 23 PFASs standard curves were all 0.2-50.0 μg · L , with
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detection limits in the range of 0.01-0.02 μg · kg . Test for recovery was made by the standard addition method, giving results in
the range of 75.8%-110%, with RSDs (n=6) of the determined values less than 7.0%. This method was used for the analysis of
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actual fish samples, and the total detection amounts of PFASs were in the range of 0.039-1.310 μg · kg .
Keywords: ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS); perfluorinated and
polyfluoroalkyl substance; fish

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