Simultaneous determination of sulpiride and its alkaline degradation product by second derivative synchronous fluorescence spectroscopy

Simple and sensitive synchronous fluori metric, and second derivative synchronous fluorometric methods were developed for the validated and simultaneous determination of sulpiride (SLP) and its alkaline degradation product (DSLP). The method is based on measuring the synchronous fluorescence of both the drug and its degradation product in borate buffer of pH 8 at A) of 45 nm. The peak amplitude (D-2) was measured at 295.5 and 342 nm for SLP and DSLP, respectively. The different experimental parameters affecting the synchronous fluorescence intensity of both compounds were studied and optimized. The fluorescence-concentration plots were rectilinear over the range of 0.05-1.0 and 2-10 mu g mL(-1) for SLP and DSLP, respectively. The limits of detection (LOD) were 0.02 and 0.4 mu g mL(-1) and quantification limits (LOQs) were 0.05 and 1.2 mu g mL(-1) for SLP and DSLP, respectively. The proposed methods were successfully applied to commercial capsules and tablets. Statistical comparison of the results with those of the official method revealed good agreement and proved that there were no significant difference in the accuracy and precision between the two methods, respectively. The method was utilized to study the kinetics of the alkaline induced degradation of the drug. The application was further extended to include the in vivo and in vitro determination of sulpiride. The mean % recoveries (n = 3)were 100.22 +/- 2.04 and 92.00 +/- 3.00 for spiked and real human plasma, respectively. (C) 2009 Elsevier B.V. All rights reserved.