title: Spectrofluorimetric method for the determination of sulpiride in pharmaceutical preparations and human plasma through derivatization with 2-cyanoacetamide.
abstract: A sensitive and accurate spectrofluorimetric method has been developed for the determination of sulpiride in pharmaceutical preparations and human plasma. The developed method is based on the derivatization reaction of 2-cyanoacetamide with sulpiride in 30% ammonical solution. The fluorescent derivatized reaction product exhibited maximum fluorescence intensity at 379 nm after excitation at 330 nm. The optimum conditions for derivatization reactions were studied and the fluorescence intensity versus concentration plot was found to be linear over the concentration range 0.2-20.0 µg/mL with a correlation coefficient of 0.9985. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.82 and 2.73 ng/mL, respectively. The proposed method was validated according to ICH guidelines. The effects of common excipients and co-administered drugs were also studied. The accuracy of the method was checked using the standard addition method and percent recoveries were found to be in the range of 99.00-101.25% for pharmaceutical preparations and 97.00-97.80% for spiked human plasma. The method was successfully applied to commercial formulations and the results obtained for the proposed method were compared with a high-performance liquid chromatography reference method and statistically evaluated using the Student's t-test for accuracy and the variance ratio F-test for precision. A reaction pathway was also proposed.
authors.affiliation: Institute of Chemical Sciences, University of Peshawar, Pakistan.
authors.forename: Jasmin
authors.initials: J
authors.lastname: Shah
authors.forename: M Rasul
authors.initials: MR
authors.lastname: Jan
authors.forename: M Naeem
authors.initials: MN
authors.lastname: Khan
authors.forename: Sultan
authors.initials: S
authors.lastname: Shah
mesh_terms: D000641:Ammonia / Q000737:chemistry; D006801:Humans; D015394:Molecular Structure; D009570:Nitriles / Q000737:chemistry*; D004364:Pharmaceutical Preparations / Q000737:chemistry*; D013050:Spectrometry, Fluorescence; D013469:Sulpiride / Q000032:analysis*; D013696:Temperature; D013997:Time Factors
chemical_list: D009570:Nitriles; D004364:Pharmaceutical Preparations; D000641:Ammonia; D013469:Sulpiride; C031594:2-cyanoacetamide