scholarly journals HPLC determination of Escitalopram in tablet dosage forms

Pharmacia ◽  
2022 ◽  
Vol 69 (1) ◽  
pp. 21-24
Author(s):  
Stefan Balkanski

Purpose: A simple, specific, precise, and accurate reversed phase liquid chromatographic (RP-LC) method has been developed for the determination of Escitalopram in tablet dosage form. Methods: The chromatographic separation was achieved on a LiChrosorb C18, 250 mm x 4.6 mm, 5 μm column at a detector wavelength of 270 nm and a flow rate of 1.0 ml/min. The mobile phase was composed of methanol, acetonitrile (70:30 v/v). The retention time of Escitalopram was 5.49 min. The method was validated for the parameters like specificity, linearity, precision, accuracy, limit of quantitation and limit of detection. Results: The method was found to be specific as no other peaks of impurities and excipients were observed. The square of correlation coefficient (R2) was 0.9999 while relative standard deviations were found to be <2.0%. Conclusion: The proposed RP-LC method can be applied for the routine analysis of commercially available formulations of Escitalopram.

Author(s):  
B. Mounika ◽  
L. Srikanth ◽  
A. Venkatesha

Objective: A reversed phase liquid chromatography was determined and validated for the estimation of Mirabegron in tablet dosage form.Methods: The validation study of RP-HPLC showed a simple, rapid, accurate, precise, reproducible results by using a stationary phase: Waters Acquity HSS T-3 C18 (100 × 2.1 mm, 1.7μm and Mobile Phase-Potassium di-hydrogen phosphate: acetone in the ratio (40:60 v/v) at PH6.0±0.02. Detection is carried out at 243 nm using UV detector.Results: The total chromatographic analysis time per sample was about 6 min with Mirabegron eluting at a retention time of 2.754. Tailing factor obtained from the standard injection is 1.6. Theoretical Plates obtained from the standard injection is 2736.7. The flow rate is 1 ml/min and linearity in the concentration range of 30-70μg/ml (R2=0.999). The precision was 0.4% the intermediate precision was 0.08%. The deliberately varied chromatographic conditions in the concentration range for the evaluation of robustness is 10-50 µg/ml, (n=3). The limit of detection (LOD) and limit of quantitation (LOQ) for Mirabegron were 0.01µg/ml and 0.05µg/ml respectively. The % recovery is 99.8 % with % R. SD of 0.09. The results proved that the optimized HPLC method fulfills these requirements within the ICH accepted limits.Conclusion: The high recovery and low relative standard deviation confirm the suitability of the proposed method for the determination of Mirabegron in tablet dosage form. 


2009 ◽  
Vol 6 (2) ◽  
pp. 489-494 ◽  
Author(s):  
B. Prasanna Kumar Reddy ◽  
Y. Ramanjaneya Reddy ◽  
D. Ramachandran

A simple, sensitive and precise high performance liquid chromatographic method for the analysis of pantoprazole sodium and lansoprazole has been developed, validated and used for the determination of compounds in commercial pharmaceutical products. The compounds were well separated an isocratically on a C18column [Inertsil C18, 5μ, 150 mm x 4.6 mm] utilizing a mobile phase consisting of acetonitrile: phosphate buffer (60:40, v/v, pH 7.0) at a flow rate of 1.0 mL/min with UV detection at 230 nm. The retention time of pantoprazole sodium and lansoprazole was found to be 2.017 min and 2.538. The procedure was validated for linearity (Correlation coefficient=0.999). The study showed that reversed-phase liquid chromatography is sensitive and selective for the determination of pantoprazole sodium and lansoprazole using single mobile phase.


2004 ◽  
Vol 87 (3) ◽  
pp. 569-572 ◽  
Author(s):  
Priyankar Ghosh ◽  
Mudiam Mohanakrishna Reddy ◽  
Beedu Sashidhar Rao ◽  
Rajendra Kumar Sarin

Abstract An analytical procedure was developed for the detection and quantitation of diazepam in cream biscuits, which were used to commit crime. The method involves the extraction of diazepam with ethanol at room temperature, and the extract is filtered, evaporated to dryness, and redissolved in the mobile phase, methanol–acetonitrile–tetrahydrofuran–water (15 + 55 + 4 + 26, v/v). The separation is achieved on a C18 reversed-phase column with the mobile phase and diode array detection (λmax) at 230 nm. Medazepam is used as the internal standard is for quantification. The calibration plot for the determination of diazepam is based on linear regression analysis (y = 0.6687x + 0.0372; r2 = 0.995). The limit of detection for diazepam in the biscuit samples was estimated as 600 ng/mL. The limit of quantitation for diazepam was estimated as 1.75 μg/mL. The diazepam detected per piece of biscuit was found to be in the range of 0.27–0.45 mg. Pure diazepam was added to biscuit samples at 3 levels (100 and 500 μg/g, and 1 mg/g), and the recoveries were found to be 95%. The mean retention time of diazepam was 2.7 min and that of medazepam (IS) was 4 min. The relative standard deviations of the diazepam level in the biscuit samples were estimated to be 0.4% for retention time and 1.02% for peak area in intraday analysis, whereas the corresponding values were and 0.61 and 2.34% in interday analysis. The method is rapid and reliable for qualitative and quantitative analysis of cream biscuits laced with diazepam, and it can be used by law enforcement laboratories for routine analysis.


1996 ◽  
Vol 79 (5) ◽  
pp. 1158-1161 ◽  
Author(s):  
Janice A Cobin ◽  
Nelson A Johnson

Abstract A liquid chromatographic method was developed and validated for determination of avermectin Bi and 8,9-Z-avermectin B1 residues in wine. The sample is extracted with hexane-acetonitrile and the hexane layer containing the avermectins is concentrated/ purified on an aminopropyl solid-phase extraction (SPE) column. The purified extract is derivatized with trifluoroacetic anhydride and the derivatized avermectins are analyzed by reversed-phase liquid chromatography with fluorescence detection. Recoveries of avermectins from wine fortified with approximately 1-25 ng/g avermectin B1a or 8,9-Zavermectin B1a averaged 88 and 102%, respectively. The limit of quantitation is 1 ng/g (signal-to-noise ratio [S/N] > 10) and the limit of detection is 0.5 ng/g (S/N > 3) for each analyte. This procedure provides a simple, rapid, and sensitive method for monitoring the total amount of avermectin residues in wine.


2012 ◽  
Vol 2012 ◽  
pp. 1-8 ◽  
Author(s):  
Snehal J. More ◽  
Suparna S. Tandulwadkar ◽  
Ajinkya R. Nikam ◽  
Atul S. Rathore ◽  
L. Sathiyanarayanan ◽  
...  

A simple, precise, and accurate reversed-phase liquid chromatographic method has been developed for the simultaneous determination of paracetamol (PCM), chlorzoxazone (CHZ), and nimesulide (NIM) in pharmaceutical dosage form. The chromatographic separation was achieved on a Thermo Hypersil GOLD C18 column (250 × 4.6 mm i.d., 5 μm particle size). The mobile phase consisted of water : acetonitrile (55 : 45 v/v). The flow rate was set to 1.2 mL min−1 and UV detection was carried out at 275 nm. The retention time () for PCM, CHZ, and NIM was found to be 2.69 ± 0.02, 4.61 ± 0.01, and 9.55 ± 0.02 min, respectively. The validation of the proposed method was carried out for linearity, precision, robustness, limit of detection, limit of quantitation, specificity, and accuracy. The linear dynamic ranges were 32.5–65.0 μg mL−1 for PCM, 37.5–75.0 μg mL−1 for CHZ, and 10.0–20.0 μg mL−1 for NIM. The developed method can be used for routine quality control analysis of titled drugs in pharmaceutical dosage form.


Molecules ◽  
2020 ◽  
Vol 25 (20) ◽  
pp. 4611
Author(s):  
Essam Ezzeldin ◽  
Nisreen F. Abo-Talib ◽  
Marwa H. Tammam ◽  
Yousif A. Asiri ◽  
Abd El-Galil E. Amr ◽  
...  

A simple, rapid, sensitive, and precise reversed-phase liquid chromatographic method was developed and validated for the simultaneous determination of four direct-acting antivirals, sofosbuvir (SF), ledipasvir (LD), declatasvir (DC), and simeprevir (SM), in their respective pharmaceutical formulations. Effective chromatographic separation was achieved on an Agilent Eclipse plus C8 column (250 mm × 4.6 mm, 5 µm) at 40 °C with gradient elution using a mobile phase composed of acetonitrile:phosphate buffer (pH 6.5). The quantification of SF and DC was based on peak area measurements at 260 nm, while the quantification of LD and SM was achieved at 330 nm. The linearity was acceptable from 1.0 to 20.0 μg/mL for the studied drugs, with correlation coefficients >0.999. The analytical performance of the newly proposed HPLC procedure was thoroughly validated according to ICH guidelines in terms of linearity, precision (RSD%, 0.39–1.57), accuracy (98.05–101.90%), specificity, limit of detection (LOD) (0.022–0.039 μg/mL), limit of quantification (LOQ) (0.067–0.118 μg/mL), and robustness. The validated HPLC method was successfully used to analyze the abovementioned drugs in their pure and dosage forms without interference from common excipients present in commercial formulations.


2019 ◽  
Vol 31 (5) ◽  
pp. 1002-1008
Author(s):  
Somana Siva Prasad ◽  
G.V. Krishna Mohan ◽  
A. Naga Babu

A novel reversed-phase high performance liquid chromatographic (HPLC) technique for the determination of everolimus (Isomer-B) and its impurities in the tablet dosage form has been optimized using analytical quality by design (QbD) approach. All the compounds are monitored with the photodiode array (PDA) detector at 280 nm and the parameters namely; precision, accuracy, specificity, stability, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The quantitation limits of IMP-A, IMP-B, IMP-C, IMP-D, IMP-E, Sirolimus and TGR are found to be 0.08, 0.08, 0.10, 0.10, 0.10, 0.08 and 0.08, respectively. Recovery studies from 0.9 mg/L to 9.0 mg/L are performed for all impurities and the values were obtained between 85-110 %. Injection volume and test concentrations have been optimized to achieve LOQ values under the reporting threshold. The whole technique is developed and validated as per International Council for Harmonization (ICH) guidelines. The proposed method is robust, sensitive, rapid and successful and helpful in the regions where regulatory agencies recommend HPLC analytical method.


2001 ◽  
Vol 84 (3) ◽  
pp. 676-683 ◽  
Author(s):  
Natividad Ramos-Martos ◽  
Francisco Aguirre-Gómez ◽  
Antonio Molina-Díaz ◽  
Luis F Capitán-Vallvey

Abstract This paper describes a rapid reversed-phase liquid chromatographic method, with UV detection, for the simultaneous determination of acetylsalicylic acid, caffeine, codeine, paracetamol, pyridoxine, and thiamine in pharmaceutical preparations. A reversed-phase C18 Nucleosil column is used. The mobile phase consists of 2 successive eluants: water (5 min) and acetonitrile–water (75 + 25, v/v; 9 min), both adjusted to pH 2.1 with phosphoric acid. Before determination acetylsalicylic acid is completely converted to salicylic acid by alkaline hydrolysis. Salicylic acid, caffeine, paracetamol, pyridoxine, and thiamine are all detected at 285 nm, whereas codeine is detected at 240 nm. Calibration curves were linear for salicylic acid, caffeine, paracetamol, and pyridoxine in the range of 50–500 mg/L, and for codeine and thiamine in the range of 50–1000 mg/L. The method was applied to the analysis of 13 fortified commercial pharmaceutical preparations. Recoveries ranged from 92.6 to 105.5%, with relative standard deviations of 1.1–5.8%.


2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.


Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.


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