title: Validated spectrofluorimetric method for determination of sulpiride in commercial formulations using Hantzsch condensation reaction.
abstract: A simple, sensitive, selective and cost effective spectrofluorimetric method has been established for the quantification of sulpiride after their complete alkaline hydrolysis. The method is based on the condensation of the primary amino group of alkaline hydrolytic product of sulpiride with acetyl acetone and formaldehyde in acidic medium (0.25 M HCl) to form a fluorescent product. The reaction product formed shows maximum fluorescence intensity at 483 nm after excitation at 431 nm. The different reaction conditions influencing the condensation reaction were carefully optimized and a linear range of 0.1-3.5 µg mL-1 with good correlation coefficient between flourescent intensity and concentration of sulpiride was found at optimum parameters. The LOD and LOQ were found to be 11 and 39 ng mL-1 respectively. The proposed method was successfully used for the quantification of sulpiride in bulk powder and commercial formulations. The effect of common pharmaceutical excipients and co-administered drug was also studied and no interferences were observed. The validity of the method was tested by analyzing sulpiride in bulk powder, and pharmaceutical formulations through recovery studies. Recoveries (%) were obtained from 98.62 to 100.24% for bulk powder, and 97.09 to 100.57 % for commercial formulations. The results were validated statistically with those obtained by reference literature high performance liquid chromatographic method.
authors.affiliation: Institute of Chemical Sciences, University of Peshawar, Peshawar, Pakistan.
authors.forename: Jasmin
authors.initials: J
authors.lastname: Shah
authors.forename: Muhammad Rasul
authors.initials: MR
authors.lastname: Jan
authors.forename: Muhammad Naeem
authors.initials: MN
authors.lastname: Khan
authors.forename: Sultan
authors.initials: S
authors.lastname: Shah
mesh_terms: D002138:Calibration; D002626:Chemistry, Pharmaceutical; D005079:Excipients / Q000737:chemistry; D005557:Formaldehyde / Q000737:chemistry; D006863:Hydrogen-Ion Concentration; D010422:Pentanones / Q000737:chemistry; D011208:Powders; D012015:Reference Standards; D015203:Reproducibility of Results; D013050:Spectrometry, Fluorescence / Q000592:standards; D013469:Sulpiride / Q000032:analysis*; D013678:Technology, Pharmaceutical / Q000379:methods* / Q000592:standards; D013696:Temperature
chemical_list: D005079:Excipients; D010422:Pentanones; D011208:Powders; D005557:Formaldehyde; C008790:acetylacetone; D013469:Sulpiride