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Peer-reviewedCC BYAnalytical chemistry

Fully Automated Purification of Small Molecules Using Online MicroSPE-UPLC-SPE.

  • Venkata Ganesh Jarubula1
  • Gerd Grewing2
  • Pauline Stark1
  • Maximilian Frey3,4
  • Dario Esposto3
  • Simon Isfort3
  • Marvin Hempel3
  • Guillaume Patoine1
  • Henriette Uthe1
  • Alain Tissier3
  • Gerd U Balcke1
4 affiliations
  1. 1Leibniz Institute of Plant Biochemistry , Program Center MetaCom, Weinberg 3, Halle/S.D-06120, Germany.
  2. 2Axel Semrau GmbH , Stefansbecke 42, SprockhövelD-45549, Germany.
  3. 3Leibniz Institute of Plant Biochemistry, Department of Cell and Metabolic Biology, Weinberg 3, Halle/S.D-06120, Germany.
  4. 4Heidelberg University, Biochemistry Center, Heidelberg69120, Germany.
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Abstract

Structural annotation of metabolites remains a key challenge in metabolomics, as NMR-based structure elucidation for every unknown UPLC peak is limited by low sensitivity and time-consuming purification. To overcome these constraints, we developed an online microSPE-UPLC platform that enables fully automated, high-throughput peak fractionation. The system allows the injection of up to 1 mL of organic extract onto microSPE cartridges in a 96-well format for metabolite enrichment and cleanup. A dual-pump loading and refocusing strategy ensures quantitative transfer to UPLC, maintaining high chromatographic resolution while collecting narrow fractions on postcolumn microSPE. Fractions can be directly eluted with deuterated solvents for NMR analysis, eliminating drying steps and preserving volatile compounds. This approach enables milligram-scale isolation of natural products per compound within a single day. The workflow was validated using plant and fungal extracts, enabling the successful purification and characterization of several sesquiterpenoids and a diterpenoid.

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Cite

BibTeXRIS
BibTeX
@article{jarubula2026fully,
  title = {{Fully Automated Purification of Small Molecules Using Online MicroSPE-UPLC-SPE.}},
  author = {Venkata Ganesh Jarubula and Gerd Grewing and Pauline Stark and Maximilian Frey and Dario Esposto and Simon Isfort and Marvin Hempel and Guillaume Patoine and Henriette Uthe and Alain Tissier and Gerd U Balcke},
  journal = {Analytical chemistry},
  year = {2026},
  month = sep,
  doi = {10.1021/acs.analchem.6c00842},
  url = {https://europepmc.org/article/MED/42916386},
  note = {CC BY},
}
RIS
TY  - JOUR
TI  - Fully Automated Purification of Small Molecules Using Online MicroSPE-UPLC-SPE.
AU  - Venkata Ganesh Jarubula
AU  - Gerd Grewing
AU  - Pauline Stark
AU  - Maximilian Frey
AU  - Dario Esposto
AU  - Simon Isfort
AU  - Marvin Hempel
AU  - Guillaume Patoine
AU  - Henriette Uthe
AU  - Alain Tissier
AU  - Gerd U Balcke
PY  - 2026
DA  - 2026/09/01
JO  - Analytical chemistry
DO  - 10.1021/acs.analchem.6c00842
UR  - https://europepmc.org/article/MED/42916386
AB  - Structural annotation of metabolites remains a key challenge in metabolomics, as NMR-based structure elucidation for every unknown UPLC peak is limited by low sensitivity and time-consuming purification. To overcome these constraints, we developed an online microSPE-UPLC platform that enables fully automated, high-throughput peak fractionation. The system allows the injection of up to 1 mL of organic extract onto microSPE cartridges in a 96-well format for metabolite enrichment and cleanup. A dual-pump loading and refocusing strategy ensures quantitative transfer to UPLC, maintaining high chromatographic resolution while collecting narrow fractions on postcolumn microSPE. Fractions can be directly eluted with deuterated solvents for NMR analysis, eliminating drying steps and preserving volatile compounds. This approach enables milligram-scale isolation of natural products per compound within a single day. The workflow was validated using plant and fungal extracts, enabling the successful purification and characterization of several sesquiterpenoids and a diterpenoid.
SN  - 0003-2700
SN  - 1520-6882
ER  -