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Development of a generic method to the solid-phase extraction of acidic compounds from complex matrices.

D M Boland1, M F Burke, T Mitchell

  • 1Department of Chemistry, University of Arizona, Tucson 85721, USA.

Journal of Analytical Toxicology
|October 16, 2001
PubMed
Summary

This study developed a mixed-mode solid-phase extraction method for purifying acidic drugs from urine. The method achieved over 80% recovery, demonstrating its effectiveness for complex biological samples.

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Area of Science:

  • Analytical Chemistry
  • Pharmacology
  • Biochemistry

Background:

  • Isolation and purification of acidic compounds from biological matrices are challenging.
  • Existing methods may lack efficiency or specificity for acidic drug analysis.

Purpose of the Study:

  • To develop and optimize a mixed-mode solid-phase extraction (SPE) procedure.
  • To enhance the isolation and purification of acidic compounds from complex biological samples, such as urine.

Main Methods:

  • Utilized Isolute HAX mixed-mode SPE columns combining hydrophobic and ion-exchange properties.
  • Optimized conditioning, sample loading, rinsing, and elution steps using specific buffers and solvent ratios.
  • Analyzed eluted acidic drugs using high-performance liquid chromatography (HPLC).

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Main Results:

  • Achieved absolute recoveries exceeding 80% for most tested acidic drugs at 1 microg/mL.
  • Demonstrated superior analyte retention and extract purity compared to separate hydrophobic or ion-exchange sorbents.
  • Identified acetate as a crucial counter-anion for optimal retention on anion-exchange columns.

Conclusions:

  • The developed mixed-mode SPE procedure is effective for purifying acidic compounds from biological matrices.
  • The choice of counter-ion significantly impacts the retention of acidic analytes in SPE.
  • This method provides a robust approach for the analysis of acidic drugs in complex samples.