In this work is presented a method for simultaneous determination of paracetamol (PA), acetylsalicylic acid (ASA) and caffeine (CA) in pharmaceutical tablets, using a bare boron‐doped diamond working electrode (BDDE) coupled to batch injection analysis system with multiple pulse amperometric detection (BIA‐MPA). The optimized sequence of fast potential pulses were applied on BDDE for acquisition of independent amperograms: +1.0 V for PA oxidation, +1.3 V for oxidation of PA and salicylic acid (SA) generated from a previous alkaline hydrolysis of ASA and +1.6 V in which the three analytes are oxidized (PA, SA and CA). Selective determination of PA is performed using the currents obtained at +1.0 V, while SA and CA signals are indirectly obtained using simple subtraction operations between peak currents from each amperogram and correction factors (CF's). The limitations of such approach on the precision and accuracy as function of BIA‐MPA conditions are discussed. Simultaneous determination of the target drugs in pharmaceutical tablets was performed by BIA‐MPA and the results compared to a HPLC‐DAD method. Under optimized conditions, the proposed method exhibits fast responses (180 injections per hour for the simultaneous determination of the three analytes) and suitable precision (RSDPA: 0.78 %; RSDSA: 1.09 %; RSDCA: 2.73 %). BIA‐MPA method is simple, portable and presents relative low‐cost.
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