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Versatile injector for inline renewable solid-phase extraction: Application to cyclodextrin-based bioaccessibility

David J Cocovi-Solberg1, Stephan Schnidrig2, Manuel Miró3

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Summary
This summary is machine-generated.

This study introduces a novel inline bead injection (BI) system for high-performance liquid chromatography (HPLC) that automates sorbent exchange. This cost-effective method enhances sample preparation by using bulk sorbents, improving efficiency and reducing waste.

Keywords:
Bead injectionInjectorInline solid-phase extractionRenewable solid-phase extractionValve

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Area of Science:

  • Analytical Chemistry
  • Chromatography
  • Sample Preparation

Background:

  • Solid phase extraction (SPE) is crucial for HPLC sample preparation but faces challenges with inline cartridges like irreversible sorption and compaction.
  • Bead injection (BI) offers sorbent renewal but lacks a versatile, automated tool for HPLC using inexpensive bulk sorbents.

Purpose of the Study:

  • To develop a versatile and reliable HPLC tool for automatic inline micro-solid phase extraction using bead injection.
  • To enable real-time sample processing with automated sorbent exchange for diverse bulk sorbents.

Main Methods:

  • A novel flow path for a liquid chromatographic injector was designed to perform inline micro-solid phase extraction.
  • The system automatically manipulates desired bed mass, retains it with an inline frit, and optionally removes it via forward flow.
  • Sorbent beds (ca. 3 mg) are exchanged before each run to prevent carryover, with potential application in Flow Injection Analysis.

Main Results:

  • Inline micro-SPE processes samples in real-time, trapping analytes and discarding the matrix within 70 seconds.
  • Achieved average enrichment factors of 250 after processing 3200 µL of sample in 16 minutes, maintaining peak characteristics.
  • Demonstrated chromatographic performance comparable to standard HPLC injectors and applied to monitor persistent organic contaminants in soil.

Conclusions:

  • This work presents the first automated inline BI-SPE for HPLC, allowing real-time sorbent swapping using bulk sorbents without extra hardware.
  • The developed valve autonomously exchanges sorbents in real-time, functioning as a cartridge exchanger for diverse samples.
  • This approach offers a cost-effective and environmentally friendlier alternative for automated sample preparation in HPLC and other techniques.