An eco-friendly, novel, rapid, accurate, and precise voltametric method for the determination of prucalopride succinate (PRU) in drug substance and its dosage form. The drug showed an anodic oxidation peak at a potential of 0.989 V using zirconium oxide nanoparticles modified carbon paste electrode (2% ZrO2/CPE) as a suitable electrochemical transducer in phosphate buffer of pH 6. Voltametric peaks which were diffusion-controlled, have been recorded and the experimental conditions including change in pH, different electrode modifiers, different buffer solutions, the effect of different types of surfactants and scan rates were all optimized. The peak current showed good linearity and sensitivity over the concentration range of 4.03 10 -7 to 2.20 10 -6 mol L -1 with a 0.9992 correlation coefficient. The limit of detection and limit of quantitation were found to be 9.23 10 -8 mol L -1 and 2.80  10 -7 mol L -1 , respectively. The prospective validated method was successfully used for the evaluation of (PRU) in dosage form without the interference of the excipients with recovery (%) ± % RSD of 100.52 ± 1.29. All validation parameters were measured according to ICH guidelines.

A sequential spectrophotometric resolution technique (SSRT) was developed in this study without the use of systematic separation procedures to determine drug of a quaternary combination; caffeine (CAF), pseudoephedrine (PSE), doxylamine succinate (DOX), and paracetamol (PAR). Their presence in a tablet with a gap ratio of 3:3:1:150, respectively, and their overlapping spectra with low absorptivities make their resolution and determination impossible without prior separation. successive ratio subtraction technique (SRST) and constant multiplication method were used to solve these problems. Furthermore, an in-lab sample enrichment technique was applied to increase minor components concentration and consequently their absorbanses (CAF, PSE, and DOX). The D0 absorption spectra were generated by successive ratios followed by subtraction and multiplication of the constants. The maximum absorbances of the drugs tested, namely (CAF, PSE, DOX and PAR) were measured at wavelengths of 272.0, 257.0, 260.0, and 248.0 nm, respectively. The limits of detection (LOD) and limits of quantification (LOQ) were 0.021, 0.124, 0.186, 0.137 and 0.070, 0.414, 0.621, 0.456 (µg/mL), respectively. The linearitiy ranges (µg/mL) were 1.0–22.0, 1.0–24.0, 10.0–90.0 and 1.0–15.0 for CAF, PSE, DOX, and PAR, respectively. The International Conference on Harmonization (ICH) guidelines were applied for method validation, and the results obtained were within the limited parameters. The finding results were compared to official and/or published analytical methods to determine the procedure's reliability. It was noted that there was no actual difference in accuracy and precision between both meyhods. The proposed technique is sensitive, selective and economic;so it can be applied to the simultaneous analysis of these drugs in their commercial tablets and/or in quality-control laboratories.

Cathodic voltammetric behaviors of drospirenone and ethinylestradiol were used for the simultaneous determination of both drugs in bulk and in pharmaceutical formulation (Yasmin® tablets) without the interference of excipients. The determinations were made on hanging mercury dropping electrode using square-wave technique in a voltammetric cell containing 10 mL of 0.04 mole/L Britton-Robinson. After every aliquot addition, the solution was stirred for 10 s at 1000 rpm, rested for 10 s then square wave voltammetry mode was ramped from +100 to -1700 mV with scan rate of 100 mV/s, pulse amplitude of 50 mV and measurement time of 5 ms. Several factors such as pH, type of supporting electrolyte, pulse amplitude and scan rate were studied to optimize the condition for voltammetric determination of these drugs. With optimized experimental parameters, a good linearity was obtained for both drugs over a range of 1.36×10-6 to 1.91×10-7 mole/L and 6.75×10-8 to 6.07×10-7 mol/L of drospirenone and ethinylestradiol, respectively. Characterization of the proposed method was done according to International Conference on Harmonization, Q2B: Validation of Analytical procedures. The proposed method was statistically compared with the reference method and the results revealed no significant difference regarding accuracy and precision.

No abstract

No abstract