A new simple, precise, rapid and selective HPLC-RP method has been developed for the simultaneous determination of Norfloxacin and Tinidazole in formulations, using 0.2 % Triethylamine (TEA) in water : Acetonitrile (80:20,v/v) and pH adjusted to 2.6 to 2.8 with Phosphoric acid , as a mobile phase, and C ,8 SHODEX column (5 micron, 25 cm x 3.9 mm, ID) as stationary phase. Detection was camed out using a UV detector at 3 1 1 nm Linearity range and percentage recoveries for Norfloxacin and Tinidazole were 20 -200 &mL and 30 -300 pg/mL, 99.91 % and 99.94 % respectively.
New analytical quality by design-oriented HPLC method with multiple response optimization (Derringer’s desirability function) was demonstrated for simultaneous analysis of three antidiabetic drugs (metformin hydrochloride/empagliflozin/linagliptin) in a fixed-dose combination. Central composite design was employed for systematic optimization of critical method parameters, namely, % organic phase (X1), aqueous phase pH (X2) and flow rate (X3) while resolution, capacity factor and theoretical plate number as critical analytical attributes. Effective chromatographic separation of title analytes was accomplished on Std. Discovery C18 column at 30°C with mobile phase comprising acetonitrile: phosphate buffer pH 5 (38:62% v/v), pumped at a flow rate of 1 mL/min by isocratic elution pattern and UV detection at 222 nm. The model is rectilinear in the range of 1.0–200, 0.2–40 and 0.1–20 μg/mL at retention times of 3.04, 3.93 and 5.99 min for metformin, empagliflozin and linagliptin, respectively. The method obeyed all validation parameters of ICH Q2(R1) guidelines. The proposed HPLC method was highly robust for method transfer, regulatory flexibility within design space and can be used for assay of pharmaceutical dosage forms comprising these analytes. The proposed method was applied for stability studies of drugs under various stress conditions.
A new simple, precise, rapid, and selective reversed-phase ion pair high-performance liquid chromatography (RP-HPLC) method has been developed for the simultaneous determination of pseudoephidrine (PSE) and terfanidine (TER) from tablets using 60:15:25 acetontrile:methanol:water (v/v) containing 2.9 g sodium lauryl sulfate/liter, pH adjusted to 3.1 using phosphoric acid as a mobile phase and C18 Spherisorb ODS 2 (3 microns, 5 cm x 4.6 mm i.d.) as stationary phase. Detection was carried out using a UV detector at 254 nm. A constant flow of 1.0 ml/min was maintained throughout the analysis. Retention times for PSE and TER were 1.90 and 7.35 min, respectively. Linearity range and percentage recoveries for PSE and TER were 24-1200 and 12-600 micrograms/ml, and 100.01 and 100.4%, respectively.
Background
Analytical quality by design driven HPLC method has been optimized for simultaneous estimation of dapagliflozin and saxagliptin in pharmaceutical dosage form. Response surface methodology was employed for optimization of experimental conditions using three factors such as organic phase (%), pH of aqueous phase, and flow rate of mobile phase.
Results
Virtuous separation of analytes was achieved with mobile phase consisted of acetonitrile: phosphate buffer, pH 5.8 (26:74% v/v) with flow rate 0.96 mL/min using SPOLAR C18 column (250 × 4.6 mm, 5 μ) with run time 6 min and UV detection at 236 nm. Retention time for dapagliflozin and saxagliptin were found to be 3.5 and 5.0 min, respectively. Method was validated as per ICH guidelines. The plot between peak area vs concentration for dapagliflozin and saxagliptin were rectilinear in the range of 0.2-300 μg/mL and 0.1-150 μg/mL respectively with detection and quantification limits were 0.061 and 0.18 μg/mL for dapagliflozin and 0.014 and 0.043 μg/mL for saxagliptin, respectively.
Conclusion
The proposed method was exploited for assay, in vitro dissolution, and stability studies of target drugs in marketed dosage form.
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