A rapid and simple stability-indicating liquid chromatographic method was developed and validated for analysis of mesna in the presence of its degradation products in drug substance and drug products in a run time not >5 min. The separation was achieved on a RP amide C16 column at room temperature using methanol-phosphate buffer (10:90, v/v, pH 3.0) as mobile phase at a flow rate of 1 mL min(-1) and UV detection at 210 nm. The detector response for mesna was linear over the selected concentration range from 50 to 1000 µg mL(-1) with a correlation coefficient 0.9998. The limit of detection and the limit of quantitation were 7.5 and 22.7 µg mL(-1), respectively. The solution was stable for at least 5 days. Baseline resolution between mesna and its degradation products was achieved. Diode array detection peak purity tests showed no peak interfered with mesna peak. Moreover, the method was successfully applied for the determination of mesna in two different commercially available drug products.
A sensitive, accurate and precise voltammetric method was developed and validated for the determination of a selective factor Xa inhibitor apixaban in drug substances using a multi-walled carbon nanotube-modified carbon paste electrode (MWCNT/CPE).
Sensitive, accurate and precise square-wave voltammetric method was developed and validated for determination of a new antiplatelet drug ticagrelor in drug substance using multi-walled carbon nanotubes titanium dioxide nanoparticles modified carbon paste electrode (MWCNTs/TiNPs/CPE). The electrochemical behavior of ticagrelor showed irreversible adsorption-diffusion controlled process at potential of 0.97 V in Britton Robinson buffer (pH 2.0). Various experimental conditions were investigated and optimized including different pH, buffers, electrode modifiers, scan rates and several surfactants. The diffusion coefficient was calculated using chronoamperometric technique. The peak current varied linearly over the concentration ranges from 1.00 × 10 −6 mol L −1 to 1.90 × 10 −4 mol L −1 with correlation coefficients of 0.9992. The detection and quantification limits were 2.81 × 10 −7 and 8.41 × 10 −7 mol L −1 , respectively. The method was successfully applied for the determination of ticagrelor in drug product and biological fluid. The pharmacokinetic parameters of drug in human plasma were estimated as: C max = 1.19 × 10 −6 mol L −1 , t max = 2 h, CL = 0.0024 Lh −1 and t 1/2 = 6.5 h which are favorably compared with those reported in literature.
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