Semi-automatic liquid chromatographic analysis of pamidronate in urine after derivatization with 1-naphthylisothiocyanate

J Chromatogr B Biomed Sci Appl. 1999 Jun 25;730(1):95-9. doi: 10.1016/s0378-4347(99)00196-6.

Abstract

An existing sensitive chromatographic assay for pamidronate in urine has considerably been automated. Using the same sample processor, the solid-phase extraction (SPE) was automated separately from the derivatization with 1-naphthylisothiocyanate, the two-fold ion-pair liquid-liquid-extraction and the treatment with hydrogen peroxide for the 2-20 ng/ml concentration range. The automatic procedure was preceded by a triple calcium precipitation and interrupted by evaporation of the SPE eluate under nitrogen. For the 0.5-5 microg/ml concentration range one automatic sequence was used by avoiding evaporation during the sample treatment. In addition to the labour-saving of the semi-automatic procedure, the daily sample-throughput was improved compared to the existing manual assay. Further, the validation showed marginal improvements in the precision, accuracy and lower limit of quantification.

MeSH terms

  • 1-Naphthylisothiocyanate / chemistry
  • Automation
  • Chromatography, Liquid / methods*
  • Diphosphonates / chemistry
  • Diphosphonates / pharmacokinetics
  • Diphosphonates / urine*
  • Humans
  • Indicators and Reagents / chemistry
  • Pamidronate
  • Reproducibility of Results
  • Sensitivity and Specificity

Substances

  • Diphosphonates
  • Indicators and Reagents
  • 1-Naphthylisothiocyanate
  • Pamidronate