LOU Xiao-han,TONG Yu-jun,CHENG Fei,YOU Jing.Screening of New Pollutants in Biological Samples:A Combined Purification Method Based on Dialysis and Gel Permeation Chromatography[J].Journal of Instrumental Analysis,2024,43(08):1212-1219.
LOU Xiao-han,TONG Yu-jun,CHENG Fei,YOU Jing.Screening of New Pollutants in Biological Samples:A Combined Purification Method Based on Dialysis and Gel Permeation Chromatography[J].Journal of Instrumental Analysis,2024,43(08):1212-1219. DOI: 10.12452/j.fxcsxb.24052365.
Screening of New Pollutants in Biological Samples:A Combined Purification Method Based on Dialysis and Gel Permeation Chromatography
In the present study,a cleanup method using a combination of dialysis and gel permeation chromatography(GPC) was developed to remove lipids as well as natural hormones from biological samples with the Asian clam(
Corbicula fluminea
) as the model organism. To effectively screen new pollutants across different categories in biological samples,the procedures of sample extraction,dialysis,and GPC separation were optimized. This method effectively removed lipids and other endogenous interferences from biological samples while retaining a broad range of new pollutants. We selected 35 contaminants with diverse physicochemical properties(log
K
ow
ranging from -1.30 to 8.41) and evaluated their recoveries after each processing step and measured the lipid contents throughout the entire cleanup procedure. The optimized extraction method was to use accelerated solvent extraction(ASE) with a mixture of hexane,acetone and dichloromethane(2∶2∶1,volume ratio) and acetonitrile,sequentially. The extracts were subjected to four rounds of dialysis,and then were purified using GPC. Depending on their physicochemical properties,target analytes were analyzed by gas chromatography-mass spectrometry(GC-MS) or liquid chromatography-tandem mass spectrometry(LC-MS/MS). Furthermore
,a vanillin-phosphoric acid method was applied to measure lipid content after each purification step. At the same time,removal efficiency of the interferences was also verified using chromatography-mass spectrometry analyses in scan mode. Results after the combined dialysis and GPC treatment showed the residual lipid content in sample extraction was less than 1.06%. The elution time for target analytes in GPC was determined to be between 8 to 20 min. Average recoveries was 55.1%±13.0%,with relative standard deviations of 1.4%–9.2%. In conclusion,the developed method effectively removed lipids and some endogenous substances from clam extracts. Meanwhile,the recoveries of all target analytes have met the requirements for trace environmental sample analysis,showing the feasibility of using this method to prepare biota samples for non-target analysis.
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