Neste trabalho descreve-se a determinação do ácido acetilsalicílico (ASA) em formulações farmacêuticas empregando voltametria de onda quadrada (SWV) e um eletrodo de diamante dopado com boro (BDD). Neste método, ASA é determinado diretamente em solução de H 2 SO 4 0,01 mol L -1 , sem a necessidade da hidrólise alcalina. Foi obtido um único pico de oxidação no potencial de 1,97 V vs. Ag/AgCl (KCl 3,0 mol L -1 ) com características de uma reação irreversível. A curva analítica obtida é linear na faixa de concentração ASA de 2,50 × 10 -6 -1,05 × 10 -4 mol L -1 , com um limite de detecção de 2,0 µmol L -1 . O desvio padrão relativo foi menor que 1,4% para uma solução de ASA 45 µmol L -1 (n = 10). O método proposto foi aplicado com sucesso para a determinação de ASA em várias formulações farmacêuticas e os resultados obtidos foram concordantes com um método oficial da Farmacopéia Britânica, a um nível de confiança de 95%.In this paper the determination of acetylsalicylic acid (ASA) in pharmaceutical formulations using square-wave voltammetry (SWV) and a boron-doped diamond electrode (BDD) is described. By this proposed method, ASA is directly determined in a 0.01 mol L -1 H 2 SO 4 solution without the need of a previous time-consuming alkaline hydrolysis step. A single oxidation peak at a potential of 1.97 V vs. Ag/AgCl (3.0 mol L -1 KCl) with the characteristics of an irreversible reaction was obtained. The obtained analytical curve is linear in the ASA concentration range 2.50 × 10 -6 -1.05 × 10 -4 mol L -1 , with a detection limit of 2.0 µmol L -1 . The obtained relative standard deviation was smaller than 1.4% for a 45 µmol L -1 ASA solution (n = 10). The proposed method was applied with success in the determination of ASA in several pharmaceutical formulations; the obtained results were in close agreement, at a 95% confidence level, with those obtained using an official method of the British Pharmacopoeia.Keywords: acetylsalicylic acid determination, boron-doped diamond electrode, square-wave voltammetry, pharmaceutical formulations
IntroductionAcetylsalicylic acid (ASA), shown in Figure 1, more popularly known as aspirin, is one of the oldest medicines that still plays an important role in modern therapeutics. It is widely employed in pharmaceutical formulations for the relief of headaches, fever, muscular pain, and inflammation due to arthritis or injury. It was first synthesized in 1897, by Felix Hoffmann, in the Farbenfabrik Freidrich Bayer laboratories, in Elberfeld, Germany. 1,2 The high consumption of this substance all over the world 3,4 indicates the importance of the development of new analytical methods to assess not only the quality but also the authenticity of the product.The rate of decomposition of ASA to salicylic acid (SA) and acetic acid (AA) is dependent on solution pH and temperature. In the pH range 11-12 ASA is quickly hydrolyzed, in the pH range 4-8 its hydrolysis rate is slow, and maximum stability is attained at pH 2-3. 5 Commonly, ASA is indirectly determined after its conversion to SA ...