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Related Experiment Videos

Systematic error in automated in-tube solid-phase microextraction.

Anil R Raghani1, Kristin N Schultz

  • 1Pharmacia Corporation, Global Chemical Process R&D, 4901 Searle Parkway, Skokie, IL 60077, USA. anil.r.raghani@pharmacia.com

Journal of Chromatography. A
|June 13, 2003
PubMed
Summary

Automated in-tube solid-phase microextraction (SPME) causes systematic errors due to analyte accumulation. Adding an air plug minimizes this error, improving quantitative accuracy in sample enrichment.

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Area of Science:

  • Analytical Chemistry
  • Chromatography
  • Sample Preparation

Background:

  • Automated in-tube solid-phase microextraction (SPME) is widely used for sample enrichment.
  • Commercial liquid chromatography autosamplers are often modified for automated SPME.
  • This configuration can introduce systematic errors in analyte quantitation.

Purpose of the Study:

  • To identify the source of systematic error in automated in-tube SPME.
  • To investigate the impact of analyte accumulation on quantitative accuracy.
  • To evaluate a method for mitigating this systematic error.

Main Methods:

  • Investigated analyte accumulation in autosampler components (sample loop, metering valve).
  • Analyzed the effect of residual mobile phase on analyte carryover.

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  • Quantified analyte accumulation across multiple draw/eject cycles.
  • Assessed the impact of a 100-microl air plug on systematic error.

    • Main Results:

    • Analyte accumulation in the pre-extraction and extraction segments was identified as the source of error.
    • Accumulation increased with the number of draw/eject cycles, leading to overestimation of detection and quantitation limits.
    • Sample/mobile phase mixing in these segments caused cross-contamination.
    • Insertion of a 100-microl air plug significantly minimized sample/mobile phase mixing and systematic error.

    Conclusions:

    • Automated in-tube SPME configurations using modified autosamplers are prone to systematic quantitative errors.
    • Analyte accumulation due to residual mobile phase is the primary cause of inaccuracy.
    • Employing an air plug is an effective strategy to reduce cross-contamination and improve the reliability of automated in-tube SPME.