Determinação de Sb (V) em medicamentos antileishmanioticos por extração liquido-liquido em sistema automatizado de analise em fluxo

AUTOR(ES)
DATA DE PUBLICAÇÃO

2003

RESUMO

In this work a selective method for the Sb (V) determination in antileishmaniotics drugs is proposed, based on the extraction of an ion pair formed between hexachloroantimoniate anion and the rhodamine a cation in an automated liquid-liquid extraction flow analysis system (LLE-FA). The ion-pair was formed in hydrochloride acid and as solvent toluene was employed. The extraction process was optimized and the following experimental parameters were established: volume of the extraction vessel 5 mL, 6 mol L hydrochloride acid, sample loop of 150 mL, 900 mL of rhodamine B, 100 s of stirring time, 80 s for the phase separation and 1 mL of toluene as extractor solvent. For the analyses of Sb (V) in N-meglumine antimoniate, the ultra-sound energy was required to liberate the antimony from the organostibium complex for the further ion pair formation. The evaluated parameters and results for the validation of the proposed method comprised: linear range (7.0x10 a 7.2x10 mol L Sb (V), linearity (0.9989), sensitivity (1.61x10± 2 u.a. L mol, P<0.05), repeatability (3.5 %, for 4.1x10 mol L Sb (V) (n= 5)), selectivity (As (V) interferes), limit of detection (2.9x10 mol L of Sb (V)) and limit of determination (9,6x10-5 mol L-1 de Sb (V)). The accuracy of the method was evaluated through comparison of results obtained by the analyses of drugs by the proposed LLE-FA method with those obtained by inductive coupled plasma optic emission spectrometry (ICP-OES) and differential pulse polarography for total antimony and Sb (III), respectively. The proposed rnethod presented an analytical frequency of 8-analysis h, an extraction efficiency of 50.5 % and low organic reagents consumption. The automated LLE-FA is suitable for the Sb (V) determination in the quality control of antileishmaniotics drugs.

ASSUNTO(S)

leishmaniose antimonio troca ionica

ACESSO AO ARTIGO

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