Simple and simultaneous determination of sulphapyridine and acetylsulphapyridine in human serum by column-switching high-performance liquid chromatography

J Clin Pharm Ther. 2002 Dec;27(6):403-8. doi: 10.1046/j.1365-2710.2002.00437.x.

Abstract

Objective: A high-performance liquid chromatography (HPLC) with an automated on-line column-switching system was used for the simultaneous determination of sulphapyridine and acetylsulphapyridine, two major active metabolites related to the adverse effects of sulphasalazine, in human serum.

Methods: Serum samples were directly injected into the HPLC, with the valve automatically switched on to remove serum proteins and other hydrophilic components remaining in the pre-column after elution of sulphapyridine and acetylsulphapyridine to the analytical column.

Results: Serum proteins did not interfere with the analysis of either compound. The recoveries of SLP and Ac-SLP from drug-free human serum were 93.03-99.18% and CV were 2.88-4.34%. The within-run reproducibility of assays was excellent with relative standard deviations (RSD) of 1.01-3.90% (SLP) and 0.77-5.56% (Ac-SLP). The limit of quantification of sulphapyridine and acetylsulphapyridine was 3.13 microg/mL and 0.50 microg/mL, respectively. The serum concentrations in a patient with ulcerative colitis, who took 1.0 g sulphasalazine twice daily, were 31.20 microg/mL for sulphapyridine and 14.64 microg/mL for acetylsulphapyridine at 7 h after ingestion.

Conclusion: The present simple and reproducible assay was useful for the monitoring of serum sulphapyridine and acetylsulphapyridine.

Publication types

  • Evaluation Study

MeSH terms

  • Administration, Oral
  • Anti-Inflammatory Agents, Non-Steroidal / administration & dosage
  • Anti-Inflammatory Agents, Non-Steroidal / blood
  • Anti-Inflammatory Agents, Non-Steroidal / pharmacokinetics*
  • Chromatography, High Pressure Liquid / methods*
  • Drug Monitoring / methods
  • Humans
  • Reproducibility of Results
  • Sulfapyridine / analogs & derivatives
  • Sulfapyridine / blood*
  • Sulfasalazine / administration & dosage
  • Sulfasalazine / blood
  • Sulfasalazine / pharmacokinetics*

Substances

  • Anti-Inflammatory Agents, Non-Steroidal
  • acetylsulfapyridine
  • Sulfasalazine
  • Sulfapyridine