| This paper investigated the chemiluminescence(CL) behavior of acid potassium permanganate-polyphosphoric acid-cephalosporin system while the reasonable hypothesis of chemiluminescence mechanism in this system was summarized through the discussion on the chemiluminescence spectrum characteristics. Based on this research, two novel flow-injection chemiluminescence methods with all- purpose for the determination of cephalosporins antibiotic were developed by utilizing acid potassium permanganate CL system. The proposed methods with the advantage of simplicity, rapidity and reproducibility could be satisfactorily used in the measurement of cephalosporins pharmaceuticals.This paper consists of three parts.Part One A review on the application of CL analysis in medicament determinationThis chapter mainly summarized the application of CL analysis on medicament determination in the past five years. Meanwhile, the determination mechanism was also discussed. 141 references were cited.Part Two Luminescence mechanism research of acid potassium permanganate CL systemThis chapter reviewed the mechanism research of acid potassium permanganate CL system and the different viewpoints about emitting species of potassium permanganate CL system were listed. Further, the CL spectrum of cephalosporins reacted with acid potassium permanganate was inspected and the luminescence mechanism of acid potassium permanganate CL system was proposed.Part Three Applications of acid potassium permanganate CL system inβ-lactam antibiotic in Pharmaceutical PreparationsChapter One Flow injection chemiluminescence determination of cefazolin sodium in PharmaceuticalsA novel analytical procedure for the determination of cefazolin is presented, based on the chemiluminescence reaction of the cefazolin sodium with potassium permanganate in the presence of polyphosphoric acid (PPA).Under the optimum conditions, the linear range of the method is 1.6～350μg mL-1 with a detection limit of 1.6μg mL-1. Relative standard deviation (RSD) is 0.6% for 50 mg/L cefazolin sodium(n=ll).The proposed method has been applied to the determination of cefazolin sodium in pharmaceutical with satisfactory results. The mechanism of the CL reaction has also been discussed.Chapter Two Determination of cephalosporins in pharmaceutical formulations by flow injection analysis with acid potassium permanganate chemiluminescence detectionA rapid, accurate and sensitive method has been developed and validated for the quantitative determination of five cephalosporins, cefadroxil, cefoperazone sodium, cefradine, cefalexin sodium and cefotaxime sodium This method based on the chemiluminescence reaction of the cephalosporins with potassium permanganate in polyphosphoric acid. The limits of detection estimated by a conservative model (3s) were 0.05μg mL-1 for cefadroxil, 0.1μg mL-1 for cefoperazone, 0.3μg mL-1 for cefradine, 0.7μg mL-1 for cefalexin and 1.6μg mL-1 for cefotaxime, respectively. The maximum relative standard deviation ( RSD ) of five cephalosporins was less than 0.8 %(n=11, C=20μg mL-1). The present analytical procedure was applied to the determination of cefoperazone sodium and cefotaxime sodium in dosage form with excellent recoveries.Chapter Three Flow-Injection Analysis of cephalosporins with indirect chemiluminescence methodIn this section, It was found that cephalosporins alkalescence hydrolysate oxidized by potassium permanganate could generate faint chemiluminescence(CL), polyphosphoric acid (PPA) could significantly enhance the generation of this CL. Based on above experimental fact, this paper present a simple, accurate, steady analytical procedure for the determination of cefotaxime sodium and ceftriaxone sodium. Under the optimum conditions, the relationship between the CL intensity and the concentration of are linear in the range of 0.02～120μg·mL-1 with detection limit of 20 ng mL-1 for cefotaxime sodium and 0.05μg·mL-1～100μg·mL-1 with adetection limit of 25 ng mL-1 for ceftriaxone sodium, respectively. The present analytical procedure was applied to the determination of cefotaxime sodium and ceftriaxone sodium in dosage form. The sensitivity of the proposed analytical procedure was superior to classical HPLC methods in the open literatures. |
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