Chemometric and derivative methods as flexible spectrophotometric approaches for dissolution and assaying tests in multicomponent tablets.
Two derivative spectrophotometric (ratio derivative spectra and algorithm bivariate calibration) and a chemometric methods (partial least squares, PLS) are proposed for the simultaneous determination of binary mixtures in tablet analysis and dissolutions tests, without prior separation. These approaches are successfully applied to quantify trimethoprim (TMP) combined with sulfamethoxazole (SMX) or sulfamethazine (SMZ) or sulfafurazole (SFZ) using the information in the absorption spectra of appropriate solutions. Beer's law was obeyed in the concentration range of 0.98-17.5 microg/ml for TMP, 0.95-17.2 microg/ml for SMX, 1.16-17.5 microg/ml for SMZ and 0.97-17.4 microg/ml for SFZ. The first derivative (1D) bivariate algorithm method involves the use of four calibration curves: two for each compound at two different wavelengths, selected by Kaiser's method. Similarly, the first derivative ratio spectrophotometry employs the linear relationship between the ratio spectra of the analytes and the concentration range. The results were compared with those obtained by PLS multivariate calibration. The calibration models from PLS were pre-treated by orthogonal signal correction and evaluated by cross-validation using the 'SIMCA-P 9' software. Synthetic mixtures of TMP and sulfonamides were used in five different sets for the validity of the calibrations. Mean recoveries for derivative ratio, derivative bivariate and PLS methods were found to be between 99.7% and 102.0% for TMP, 99.4% and 100.2% for SMX, 99.3% and 101.0% for SMZ and 98.1% and 102.3% for SFZ. The calibrations of the three methods were successfully applied to the assaying and dissolution of placebo and commercial tablets without any prior separation. More than 85% of TMP, SMX and SMZ were dissolved within 15 min. For SFZ, only 85% of the compound was dissolved after 60 min. In this study, the three spectrophotometric methods can be satisfactorily used for the quantitative analysis and for dissolution tests of multicomponent dosage forms.
Markopoulou
Catherine K
CK
Laboratory of Pharmaceutical Analysis, School of Pharmacy, Aristotelian University, Thessaloniki 54124, Greece. koundour@pharm.auth.gr
Malliou
Eleftheria T
ET
Koundourellis
John E
JE
D000465:Algorithms; D002138:Calibration; D002623:Chemistry Techniques, Analytical / Q000379:methods; D016018:Least-Squares Analysis; D015999:Multivariate Analysis; D015203:Reproducibility of Results; D013053:Spectrophotometry / Q000379:methods; D013418:Sulfamethazine / Q000032:analysis; D013420:Sulfamethoxazole / Q000032:analysis; D013424:Sulfanilamides / Q000032:analysis*; D013444:Sulfisoxazole / Q000032:analysis; D013607:Tablets / Q000737:chemistry*; D013678:Technology, Pharmaceutical / Q000379:methods; D013997:Time Factors; D014295:Trimethoprim / Q000032:analysis*
D013424:Sulfanilamides; D013607:Tablets; D013418:Sulfamethazine; D013444:Sulfisoxazole; D014295:Trimethoprim; D013420:Sulfamethoxazole