Flow analysis /hydride generation  /Fourier transform infrared spectrometric determination of antimony in pharmaceuticals M. Gallignani *, C. Ayala, M.R. Brunetto, M. Burguera, J.L. Burguera Venezuelan Andean Institute for Chemical Research (IVAIQUIM), Faculty of Science, University of Los Andes, P.O. Box 440, Merida 5101-A, Venezuela Received 8 July 2002; received in revised form 27 November 2002; accepted 27 November 2002 Abstract In this work, a flow analysis system with hydride generation and Fourier transform infrared (FTIR) spectrometric detection has been developed for the determination of antimony in pharmaceuticals. The method is based on the on-line mineralization/oxidation of the organic antimonials present in the sample and pre-reduction of Sb(V) to Sb(III) with K 2 S 2 O 8 and KI, respectively; prior to the stibine generation. The gaseous SbH 3 is separated from the solution in a gas phase separator, and transported by means of a nitrogen carrier into a short pathway (10 cm) IR gas cell, where the corresponding FTIR spectrum is acquired by accumulating 3 scans in a continuous mode. The 1893 cm 1 band was used for the quantification of the antimony. The procedure is carried out in a closed system, which reduces sample handling and makes possible the complete automation of the antimony determination. The figures of merit of the proposed method (linear range: 0 /600 mg l 1 , limit of detection (3s ) /0.9 mg l 1 , limit of quantification (10s ) /3 mg Sb l 1 , precision (R.S.D.) less than 1% and sample frequency /28 h 1 ), are appropriate for the designed application. Furthermore, precise and accurate results were found for the analysis of different antimonial pharmaceutical samples, indicating that the methodology developed represents a valid alternative for the determination of antimony in pharmaceuticals, which could be suitable for the routine control analysis. # 2003 Elsevier Science B.V. All rights reserved. Keywords: Antimony determination; Stibine; SbH 3 ; Glucantime; Flow analysis; Hydride generation; Fourier transform infrared spectrometry 1. Introduction Although antimony is a potentially significant element for plants, it does not have known essential function in animals; on the contrary its toxicity has been demonstrated [1,2]. However, systemic antimonial therapy is still recommended for multiple lesions caused by human leishmaniasis disease [3,4]. The toxicological and physiological behavior of this element is dependent on its oxidation state. Elemental antimony is more toxic than its salts, and trivalent antimony salts are ten times more toxic than pentavalent salts [5,6]. At present, almost all forms of leishmaniasis are * Corresponding author. Tel.:  /58-274-2401375; fax:  /58- 274-2401286. E-mail address: maximo@ula.ve (M. Gallignani). Talanta 59 (2003) 923  /934 www.elsevier.com/locate/talanta 0039-9140/03/$ - see front matter # 2003 Elsevier Science B.V. All rights reserved. doi:10.1016/S0039-9140(02)00648-3