Citation: JIN Jin, SONG Shan-Jun, PENG Zi-Juan, GUO Feng, LI Peng-Hui. Determination of Polybrominated Diphenyl Ethers and Hydroxylated Analogues in Serum Using High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry with Online Solid Phase Extraction[J]. Chinese Journal of Analytical Chemistry, ;2021, 49(4): 520-527. doi: 10.19756/j.issn.0253-3820.211074 shu

Determination of Polybrominated Diphenyl Ethers and Hydroxylated Analogues in Serum Using High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry with Online Solid Phase Extraction

JIN Jin ^1,2 ,
SONG Shan-Jun ^2,, ,
PENG Zi-Juan ² ,
GUO Feng ^3,, ,
LI Peng-Hui ¹

1.
Tianjin University of Technology, Tianjin 300384, China;
2.
National Institute of Metrology, Beijing 100029, China;
3.
National Research Center for Geoanalysis, Beijing 100037, China

Corresponding author: SONG Shan-Jun, GUO Feng,
Received Date: 26 January 2021
Revised Date: 1 March 2021

Fund Project: Supported by the National Natural Science Foundation of China (Nos.21806158, 21976044).

Online solid phase extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry (Online SPE-HPLC-ICP-MS) technique was developed for simultaneous determination of six kinds of polybrominated diphenyl ethers and five kinds of hydroxyl metabolites in serum sample. By automatic injection, 200 μL of serum sample was directly analyzed after protein precipitation and dilution. The targets in samples were automatically enriched on a solid phase extraction column, and then separated and analyzed by liquid chromatography-inductively coupled plasma mass spectrometry with methanol/acetonitrile/water mixed solvent. After optimizing the main parameters such as loading rate, elution time and elution solvent, the Oasis HLB online solid phase extraction column was finally selected. The loading solvent was pure water with a rate of 3.0 mL/min, the elution solvent was the mixture of methanol, acetonitrile and water (54:26:20, V/V), the elution flow rate was 1.0 mL/min, and the liquid chromatography column was ZORBAX Eclipse Plus C₁₈. The limits of quantification (LOQ) of the method were 0.14-0.74 ng/L, the recoveries of matrix addition were from 61.8% to 77.7%, and the relative standard deviations (RSDs) of the results were from 3.7% to 10.1% (n=3). The established method was successfully applied to the analysis of 30 serum samples. Four kinds of polybrominated diphenyl ethers and two kinds of hydroxy polybrominated diphenyl ethers were detected, and their occurrence characteristics were consistent with the previous reports. The results showed that this method could be applied to analysis and detection of large quantities of actual samples, and had a great practical value.
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