Urine iodide determination by ion-pair reversed-phase high performance liquid chromatography and pulsed amperometric detection

Talanta. 2012 Sep 15:99:532-7. doi: 10.1016/j.talanta.2012.06.028. Epub 2012 Jun 27.

Abstract

A sensitive and specific ion-pair reversed-phase high performance liquid chromatography (HPLC) method for urinary iodine analysis is described. This method is based on pulsed amperometric detection (PAD) using a silver working electrode (HPLC-PAD), which improves peak shape, electrode stability as well as linearity and reproducibility. A two-step extraction process consisting of solid phase extraction (SPE) and liquid-liquid extraction with dichloromethane was added in order to improve sample purification which is essential with the use of PAD. Treated samples were eluted on a C18 column, using a phosphate buffer containing ion-pairing reagent tetrabutylammonium and 5% MeOH. The calibration standard curves were linear up to 500 μg/L and within-run and between-run coefficients of variation (CVs) were <6% with the quantification limit fixed at 6 μg/L. Accuracy, expressed as recovery, ranged from 94% to 104%. Comparison with the Technicon AutoAnalyzer acid digestion (AA) method resulted in a high correlation (r=0.9916). Due to a low quantification limit and high sample throughput, the proposed technique appears suitable for both epidemiological and clinical follow-up studies.

MeSH terms

  • Chromatography, High Pressure Liquid / methods*
  • Chromatography, Reverse-Phase / methods*
  • Electrochemistry / instrumentation
  • Electrochemistry / methods*
  • Electrodes
  • Humans
  • Iodides / urine*
  • Limit of Detection
  • Silver / chemistry
  • Urinalysis / methods*

Substances

  • Iodides
  • Silver