Este artigo descreve um método de quimioluminescência (CL) simples, rápido e sensível para a determinação de perfenazina usando sistema de injeção em fluxo (FI). Todas as variáveis que podem afetar a resposta do método CL foram otimizadas empregando planejamento composto central (CCD) para o planejamento experimental e metodologia de superfície de resposta (RSM) para a modelagem. A otimização usando CCD comparativamente ao método univariado mostrou uma melhora significativa na sensibilidade. Sob condições experimentais ótimas, uma ampla região linear foi obtida entre a concentração do analito e a altura do pico, dentro do intervalo de 1,2 a 1.300 ng mL -1 com coeficiente de correlação de 0,9978. O limite de detecção foi de 0,4 ng mL -1(S/N = 3) e o desvio padrão relativo para 6 repetições de uma solução contendo 70,5 ng mLfoi menor que 4%. Esse método foi aplicado com sucesso na quantificação de perfenazina em formulações farmacêuticas e em soro humano com adequadas recuperações (95,3-104,0%). A frequência analítica foi de 100 ± 5 amostras por hora.This paper describes a simple, rapid and sensitive chemiluminescence (CL) method for the determination of perphenazine by flow injection (FI) system. All variables that can affect the CL response were optimized by employing central composite design (CCD) for the experimental design and response surface methodology (RSM) for the modeling. Optimization by means of CCD method with respect to conventional single factor at a time method showed a significant improvement in the sensitivity. Under the optimum experimental conditions, a wide linear relationship between analyte concentration and peak height was obtained within the range 1.2-1,300 ng mL -1 with correlation coefficient of 0.9978. The limit of detection was 0.4 ng mL -1 (S/N = 3) and the relative standard deviation for 6 repeated measurements of a solution containing 70.5 ng mL -1 was lower than 4%. This method was successfully applied for the quantification of perphenazine in pharmaceutical formulations and human serum with good recoveries (95.3-104.0%). Sample throughput was 100 ± 5 samples per hour.
Keywords: flow injection, chemiluminescence, perphenazine, central composite design
IntroductionPerphenazine belongs to the phenothiazine family of drugs. Because of its neuroleptic and antidepressive actions, it is often prescribed for the treatment of psychotic patients such as schizophrenia and schizoaffective psychoses in order to decrease restlessness, aggressiveness and impulsive behavior. Also it is found to be effectual in the treatment of Parkinson's disease. 1 The monitoring of the perphenazine is important for quality assurance in pharmaceutical industry and for obtaining optimum therapeutic concentrations in body fluids to minimize the risk of toxicity. The therapeutic range and toxic threshold of perphenazine in serum were reported 4-30 and 50-100 ng mL In experimentation, we attempt to monitor the effects of certain inputs or material on the subject matter of interest. The advantages of the experimenta...