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Untargeted Metabolomics from Biological Sources Using Ultraperformance Liquid Chromatography-High Resolution Mass Spectrometry UPLC-HRMS
Published on: May 20, 2013
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High-Throughput Solid Phase Extraction for Targeted and Nontargeted Exposomics.
Yunyun Gu1,2, Max Lennart Feuerstein1,3, Benedikt Warth1,2,3
1Faculty of Chemistry, Department of Food Chemistry and Toxicology, University of Vienna, 1090 Vienna, Austria.
Analytical Chemistry
|March 13, 2025
Summary
A new solid phase extraction (SPE) method improves chemical exposome analysis in urine and plasma. This robust, scalable protocol enhances throughput for environmental contaminant detection, aiding exposome-wide association studies.
Area of Science:
- Environmental chemistry
- Analytical chemistry
- Toxicology
Background:
- Characterizing the chemical exposome is crucial for understanding environmental health impacts.
- Current sample pretreatment methods for exposomics present bottlenecks in analyte coverage, robustness, and throughput.
- Advanced instrumentation like liquid chromatography-tandem mass spectrometry (LC-MS/MS) requires optimized sample preparation.
Purpose of the Study:
- To develop and optimize a robust and scalable solid phase extraction (SPE) protocol for human urine and plasma.
- To evaluate the extraction efficiency and signal suppression/enhancement for a diverse panel of environmental and food-related contaminants.
- To enhance the throughput of exposomic analysis for large-scale studies like exposome-wide association studies (ExWAS).
Main Methods:
- Developed a solid phase extraction (SPE) protocol for human urine and plasma.
- Optimized the SPE for 94 diverse environmental and food-related contaminants.
- Utilized targeted LC-MS/MS to determine extraction recoveries (RE) and signal suppression/enhancement (SSE).
- Transferred the method to a 96-well plate format for high-throughput analysis.
- Compared the SPE method with protein precipitation using NIST standard reference materials.
Main Results:
- Achieved acceptable extraction recoveries (60-140%) for over 70% of analytes.
- Attained acceptable signal suppression/enhancement (60-140%) for 86% of analytes in urine and 90% in plasma.
- The 96-well plate format significantly increased throughput, estimated to be ~10x faster than protein precipitation for 1000 samples.
- The SPE protocol demonstrated promising performance for nontargeted analysis (NTA) and suspect screening.
Conclusions:
- The developed SPE workflow is robust, scalable, and significantly improves throughput for targeted exposomics.
- This method offers a viable option for nontargeted analysis (NTA) and suspect screening in exposomics.
- The optimized protocol is applicable to various research fields including pharmacology, food safety, and systems toxicology.
