An improved leaping detector for flow analysis applied to iron speciation in drugs

Abstract

A low inner volume (ca. 64 ml) probe was built up in an injectorcommutator in order to behave as a photometric leaping detector in ow analysis. It comprises a bicolour lig ht-emitting diode (BLED ), as a source of pulsed radiation in the red and green visible region, and two phototransistors as transducers. Sample injection, detector relocation, analytical signal recording, data treatment and de nition of the spectral working range were computer-controlled. T he feasibility of the system was initially demonstrated in the ow-injection speciation of iron, and the overall standard deviation of results was estimated as §1.6 and §1.4% for 1.6-4.0 mg l ¡1 Fe(II) or total iron after eightfold processing of synthetic samples. T he system was further applied to drug analysis: the mean deviations of results for typical samples were estimated as §5.2 and §3.3% , and the relative standard deviation as §1.6 and §1.3% for Fe(II) and total iron, respectively. Results were compared with those obtained by a conventional spectrophotometric procedure and no statistic diå erences at the 95% con dence level were found. In relation to an earlier system with multi-site detection, the proposed system is more stable, presenting low drift with a relative standard deviation of 0.026% and 0.039% for measurements (nˆ120 during 4 h of observation) with green and red emission. It is also faster with a sampling rate of 133 h ¡1 and carryover problems are not found. T he possibility of compensating the Schlieren noise by dualwavelength spectrophotometry is discussed.