scholarly journals In Vitro Dissolution Study of Acetylsalicylic Acid and Clopidogrel Bisulfate Solid Dispersions: Validation of the RP-HPLC Method for Simultaneous Analysis

2020 ◽  
Vol 10 (14) ◽  
pp. 4792 ◽  
Author(s):  
Ehlimana Osmanović Omerdić ◽  
Larisa Alagić-Džambić ◽  
Marko Krstić ◽  
Maja Pašić-Kulenović ◽  
Jadranka Odović ◽  
...  

Solid dispersions were prepared via a solvent evaporation method, employing ethanol (96%, v/v) as solvent, with three different polymers as carrier: povidone, copovidone, and poloxamer 407. Previously developed reversed-phase HPLC (RP-HPLC) methods were modified and used for the simultaneous determination of acetylsalicylic acid and clopidogrel bisulfate and after release from solid dispersions. Chromatography was carried out on a C-18 column, with a mobile phase of acetonitrile–methanol–phosphate buffer pH 3.0, UV detection at 240 nm, and a run time of 6 min. The method was validated according to International Conference of Harmonisation guidelines and validation included specificity, accuracy, precision, linearity, robustness, limit of detection (LOD), and limit of quantification (LOQ). The method is specific for determination of acetylsalicylic acid and clopidogrel bisulfate. The linearity was provided in the concentration range 0.0275–0.1375 mg/mL for acetylsalicylic acid and 0.0200–0.1000 mg/mL for clopidogrel bisulfate, with a correlation coefficient (R2 value) of 0.9999 for both active pharmaceutical ingredients (APIs). Accuracy was confirmed by calculated recoveries for acetylsalicylic acid (98.6–101.0%) and clopidogrel bisulfate (100.0–101.6%). The intra-day and the inter-day precision-calculated relative standard deviations are less than 1%, which indicates high precision of the method. The limits of detection and quantification for acetylsalicylic acid were 0.0004 and 0.0012 mg/mL, and for clopidogrel bisulfate 0.0002 mg/mL and 0.0007 mg/mL, respectively. Small variations in chromatographic conditions did not significantly affect qualitative and quantitative system responses, which proved robustness of method. The proposed RP-HPLC method was applied for simultaneous determination of clopidogrel bisulfate and acetylsalicylic acid from solid dispersions.

Author(s):  
Shishir Tandon ◽  
Suman Lata Pal

Abstract A sensitive and reliable method for simultaneous determination of oryzalin and ethofumesate residues in pantnagar soil and water was validated. The compounds were extracted by LLE with dichloromethane from water, and acetone:methanol mixture from soil followed by SPE cleanup. Detection and quantification was done by RP-HPLC using mobile phase methanol:water (70:30, v/v) at 280 nm. The developed method showed satisfactory validation results with linearity (0.99), relative standard deviations (1.55 and 1.73%), and limit of quantification (0.002 μg g−1 and 0.005 μg g−1) for ethofumesate and oryzalin, respectively. Recoveries ranged for oryzalin and ethofumesate from 79.80–90.52, 75.58–86.04% (soil) and 83.50–95.92, 82.28–94.60% (water), respectively. The method could be used for routine high-throughput detection and determination of these compounds.


2011 ◽  
Vol 39 (05) ◽  
pp. 1043-1060 ◽  
Author(s):  
Cheng-Cheng Cai ◽  
Ma-Cheng Yan ◽  
Hui Xie ◽  
Sheng-Li Pan

Piper is a genus that is recently valued for the treatment of central nervous system diseases. The major constituents, amides and lignans, are responsible for the antinociceptive and antidepressant activities. This study developed a RP-HPLC-UV method for the simultaneous determination of eight amides and two lignans in twelve different species of Piper. HPLC separation was accomplished on a C18 analytical column (5 μm, 250 mm × 4.6 mm, i.d.) with a gradient mobile phase consisting of acetonitrile and water at a flow rate of 1.0 ml/min. All the calibration curves showed good linear correlation coefficients (r > 0.9997) over the test ranges. The relative standard deviation of the current method was less than 2.90% for intra- and inter-day assays and the average recoveries were between 98.25% and 103.08%. The HPLC method established is appropriate for quality control purposes and allows for the differentiation of Piper species.


2020 ◽  
Vol 32 (1) ◽  
pp. 39-43
Author(s):  
Abdul Shakoor ◽  
Mahmood Ahmed ◽  
Rabia Ikram ◽  
Sajad Hussain ◽  
Arifa Tahir ◽  
...  

The present work aimed to develop and validate a simple, rapid, sensitive, accurate, and precise method for simultaneous determination of metformin hydrochloride and vildagliptin in tablet and biological samples. Isocratic elution of both the analytes was performed at 35 °C by injecting 20 μL into Thermo Hypersil ODS C18 column (5 μm, 4.6 mm× 250 mm), while the flow rate was set to 0.8 mL/min. The mobile phase comprised of methanol, acetonitrile, and phosphate buffer (5:30:65, v/v, pH 3.5), and wavelength was selected at 212 nm. The overall run time per sample was 7.0 min with a retention time of 3.36 and 5.41 min for metformin hydrochloride and vildagliptin, respectively. The calibration curve was linear from 10–140 μg/mL for metformin and 1–14 μg/mL for vildagliptin with a coefficient of determination (R2) ≤ 0.9919, while repeatability and reproducibility (expressed as relative standard deviation) were lower than 1.13 and 0.97%, respectively. Force degradation studies indicated a complete separation of the analytes in the presence of their degradation products providing a high degree of method specificity. The proposed reversed-phase high-performance liquid chromatography (RP-HPLC) method was demonstrated to be simple and rapid for the determination of metformin hydrochloride and vildagliptin in commercially available tablet and biological samples providing recoveries ranged between 100.13–100.29%.


2012 ◽  
Vol 2 (2) ◽  
pp. 364-367 ◽  
Author(s):  
Saida Naik Dheeravath ◽  
◽  
Kasani Ramadevi ◽  
Zilla Saraswathi ◽  
Dheeravath Maniklal ◽  
...  

Author(s):  
Hina Shamshad ◽  
Ali Sayqal ◽  
Jahan Zeb ◽  
Agha Zeeshan Mirza

Abstract A simple, accurate and precise RP-HPLC method was developed for the simultaneous determination of chloroquine, pyrimethamine and cetirizine hydrochloride concentrations in bulk drug and human serum. The assay was performed using a mobile phase of methanol: water (70:30) at pH of 2.8 ± 0.05 on the Purospher C-18 column with UV detection at 230 nm and rosuvastatin used as an internal standard. The retention times observed for chloroquine, pyrimethamine and cetirizine hydrochloride were 3.5, 2.5 and 5.5 minutes, respectively. The method was found to be specific for the assayed drugs showing a linear response in the concentration range of 1–100 μg mL−1 with coefficients of determination values of (r = 0.999). The method was developed and validated according to ICH guidelines. The method was used to monitor the serum samples and was found to be sensitive for therapeutic purposes, showing the potential to be a useful tool for routine analysis in laboratories.


2015 ◽  
Vol 60 (4) ◽  
pp. 2729-2733 ◽  
Author(s):  
SOHEIR ABD EL-FATAH WESHAHY ◽  
MAISSA SALEM YAAQOB ◽  
MARIANNE NEBSEN MORCOS ◽  
DINA WAHBA HASSAN ◽  
NADIA FAYEK YOUSSEF

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