Spectrophotometric Study for the Reaction of Pentoxifylline Hydrochloride with 1,2-Naphthoquinone-4-Sulphonate: Kinetics, Mechanism and Application for Development of High-Throughput Kinetic Microwell Assay for Pentoxifylline in Quality Control Laboratory  

作　　者：Ashraf M. Mahmoud Saad A. AlQahtani Ashraf M. Mahmoud;Saad A. AlQahtani(Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut, Egypt;Department of Pharmaceutical Chemistry, College of Pharmacy, Najran University, Najran, Kingdom of Saudi Arabia;Department of Clinical Pharmacy, College of Pharmacy, Najran University, Najran, Kingdom of Saudi Arabia)

机构地区：[1]Department of Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Assiut University, Assiut, Egypt [2]Department of Pharmaceutical Chemistry, College of Pharmacy, Najran University, Najran, Kingdom of Saudi Arabia [3]Department of Clinical Pharmacy, College of Pharmacy, Najran University, Najran, Kingdom of Saudi Arabia

出　　处：《American Journal of Analytical Chemistry》2016年第2期179-191,共13页美国分析化学（英文）

摘　　要：Spectrophotometric study was carried out, for the first time, to investigate the reaction between the vasodilator pentoxifylline hydrochloride (POX) and 1,2-naphthoquinone-4-sulphonate (NQS) reagent. The reaction occurs in alkaline medium to activate the nucleophilic substitution reaction producing an orange-colored product measured spectrophometrically at λ_max 472 nm. The variables affecting the reaction were carefully studied and the conditions were optimized. The kinetics of the reaction was investigated and its activation energy was found to be 0.262 cal/mol. Owing to its low activation energy, the reaction proceeded easily and was successfully used for simple and rapid assay of POX. The stoichiometry of the reaction was determined (1:1), and the reaction mechanism was suggested. To develop a high-throughput methodology used in quality control laboratory, a comparative study of the reaction using the conventional spectrophotometric versus microwell assay was applied. Under the optimum reaction conditions, the initial rate and fixed time methods were utilized for constructing the calibration graphs for determination of POX concentrations. The linear range was 10 - 120 μg/ml with good correlation coefficients (0.9987 - 0.9998). The LOD was 2.5 and 3.4 μg/ml for initial rate and fixed time methods, respectively. The intra- and inter-day accuracy and precision of the developed methods were satisfactory, where RSD was ≤3.94%. The present methods have been successfully applied to the determination of POX in its pharmaceutical tablets, and the percentage recovery values were 97.9% - 101.9%. Therefore, we strongly recommend the proposed methods for determination of POX in quality control laboratories.Spectrophotometric study was carried out, for the first time, to investigate the reaction between the vasodilator pentoxifylline hydrochloride (POX) and 1,2-naphthoquinone-4-sulphonate (NQS) reagent. The reaction occurs in alkaline medium to activate the nucleophilic substitution reaction producing an orange-colored product measured spectrophometrically at λ_max 472 nm. The variables affecting the reaction were carefully studied and the conditions were optimized. The kinetics of the reaction was investigated and its activation energy was found to be 0.262 cal/mol. Owing to its low activation energy, the reaction proceeded easily and was successfully used for simple and rapid assay of POX. The stoichiometry of the reaction was determined (1:1), and the reaction mechanism was suggested. To develop a high-throughput methodology used in quality control laboratory, a comparative study of the reaction using the conventional spectrophotometric versus microwell assay was applied. Under the optimum reaction conditions, the initial rate and fixed time methods were utilized for constructing the calibration graphs for determination of POX concentrations. The linear range was 10 - 120 μg/ml with good correlation coefficients (0.9987 - 0.9998). The LOD was 2.5 and 3.4 μg/ml for initial rate and fixed time methods, respectively. The intra- and inter-day accuracy and precision of the developed methods were satisfactory, where RSD was ≤3.94%. The present methods have been successfully applied to the determination of POX in its pharmaceutical tablets, and the percentage recovery values were 97.9% - 101.9%. Therefore, we strongly recommend the proposed methods for determination of POX in quality control laboratories.

关 键 词：Pentoxifylline HCl 1 2-Naphthoquinone-4-Sulphonate Kinetic Spectrophotometry Pharmaceutical Analysis Micro-Well Plate Reader 

分 类 号：O62[理学—有机化学]