scholarly journals Novel Isocratic RP-HPLC Method Development and Validation of Rosuvastatin and Fenofibrate in Tablets

2020 ◽  
Vol 11 (03) ◽  
pp. 343-349
Author(s):  
Chandrasekhar Kudupudi ◽  
Manikandan Ayyar
Keyword(s):  
Related Compound ◽  
Method Development ◽  
Quantitative Estimation ◽  
Gradient Elution ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Phase Gradient ◽  
Compound A ◽  
Atorvastatin Calcium ◽  
Rp Hplc

A novel, simple, selective, precise, and accurate reverse-phase high-performance liquid chromatography (RP-HPLC) gradient method was developed for the simultaneous estimation of atorvastatin and fenofibrate in the combined formulation. The drugs atorvastatin calcium and fenofibrate were separated in the presence of their impurities atorvastatin related compound H, fenofibrate related compound A, and fenofibrate related compound B. The drugs and related compounds were separated on Kromasil C18 (250 x 4.6, 5μ) with reverse-phase gradient elution. Water adjusted pH 4.0 with phosphoric acid used as a buffer in pump A and acetonitrile used as a solvent in pump B as a mobile phase with gradient elution. The flow rate was 2.0 mL/min. 254 nm was the detection wavelength. The retention times were about 4.6 minutes for fenofibrate related compound A, 5.2 minutes for atorvastatin calcium, 5.7 minutes for fenofibrate related compound B, 8.7 minutes for atorvastatin related compound H, and 17.6 minutes for fenofibrate. The linearity ranges for atorvastatin calcium and fenofibrate were 5.00 to 15.00 and 80 to 240 mcg/mL, respectively, with correlation coefficient 0.999 for both. The proposed method validated statistically with respect to system suitability, specificity, linearity, precision, accuracy, range, robustness, and ruggedness. The method was accurate, linear, precise, specific, selective, and rapid suitable for the quantitative estimation of atorvastatin and fenofibrate in tablets.

scholarly journals Novel Reverse-Phase High-Performance Liquid Chromatography (RP-HPLC) Method Development and Validation of Atorvastatin and Fenofibrate in Tablets

2020 ◽  
Vol 11 (02) ◽  
pp. 232-236
Author(s):  
Chandrasekhar Kudupudi ◽  
Manikandan Ayyar
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Related Compound ◽  
High Performance ◽  
Gradient Elution ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Compound A ◽  
Atorvastatin Calcium ◽  
Rp Hplc

A novel, simple, selective, precise, and accurate reverse-phase high-performance liquid chromatography (RP-HPLC) gradient method was developed for the simultaneous estimation of atorvastatin and fenofibrate in the combined formulation. The drugs atorvastatin calcium and fenofibrate were separated in the presence of their impurities atorvastatin related compound H, fenofibrate related compound A, and fenofibrate related compound B. The drugs and related compounds were separated on Kromasil C18 (250 x 4.6, 5μ) with reverse-phase gradient elution. Water adjusted pH 4.0 with phosphoric acid used as a buffer in pump A and acetonitrile used as a solvent in pump B as a mobile phase with gradient elution. The flow rate was 2.0 mL/min. 254 nm was the detection wavelength. The retention times were about 4.6 minutes for fenofibrate related compound A, 5.2 minutes for atorvastatin calcium, 5.7 minutes for fenofibrate related compound B, 8.7 minutes for atorvastatin related compound H, and 17.6 minutes for fenofibrate. The linearity ranges for atorvastatin calcium and fenofibrate were 5.00 to 15.00 and 80 to 240 mcg/mL, respectively, with correlation coefficient 0.999 for both. The proposed method validated statistically with respect to system suitability, specificity, linearity, precision, accuracy, range, robustness, and ruggedness. The method was accurate, linear, precise, specific, selective, and rapid suitable for the quantitative estimation of atorvastatin and fenofibrate in tablets.

scholarly journals Method Development and Validation of Stability Indicating RP-HPLC Method for Simultaneous Estimation of Escitalopram Oxalate and Clonazepam in Bulk and its Pharmaceutical Formulations

2019 ◽  
Vol 9 (1-s) ◽  
pp. 265-274
Author(s):  
Bindusar Kalia ◽  
Uttam Singh Baghel
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Plot ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Rp Hplc

This article refers to simple isocratic reverse-phase high-performance liquid chromatographic method (RP-HPLC) developed for the simultaneous quantification of Escitalopram Oxalate (EST) and Clonazepam (CZP) in active pharmaceutical ingredient and pharmaceuticals. The separation of the two drugs was attained using a C₁₈ column (250mm×4.6mm, 5µ) as a stationary phase. The mobile phase was used as a mixture of methanol; acetonitrile; and 0.05M potassium dihydrogen orthophosphate buffer (pH 4 adjusted by orthophosphoric acid) with an isocratic ratio of 40:20:40 v/v. Detection was made by using PDA detector at 210 nm. Escitalopram Oxalate (RT= 4.428 minutes) and Clonazepam (RT= 6.532 minutes) were separated in a single chromatographic run with resolution of 8.719. The calibration plot indicated good linear relationship with r2 = 0.998 for Escitalopram Oxalate in concentration range of 32 µg/ml - 48 µg/ml and r2 = 0.999 for Clonazepam in concentration range of 16 µg/ml - 24 µg/ml. The retrievals for Escitalopram Oxalate and Clonazepam were found to be 99.75% and 99.00%, respectively. The established analytical method was validated and found acceptable as per ICH guidelines for linearity, precision, accuracy, specificity, limit of detection, limit of quantification, robustness and stability. Escitalopram Oxalate and Clonazepam individually as well as in combination were exposed to different stress conditions like acid, base, thermal, photolytic and oxidation degradation and peaks of a degraded product were well determined from peaks of pure drug. This method is modest, quick and appropriate for routine quality control analysis. Keywords: Reverse Phase – HPLC; Escitalopram Oxalate; Clonazepam; Validation; Degradation study.

METHOD DEVELOPMENT FOR SIMULTANEOUS ESTIMATION OF ATORVASTATIN AND NATEGLINIDE IN COMBINED DOSAGE FORM BY UV SPECTROSCOPY.

2020 ◽  
Vol 7 (9) ◽  
pp. 16-21
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Quantitative Estimation ◽  
Uv Spectroscopy ◽  
Simultaneous Equation ◽  
Dosage Forms ◽  
Chemotherapeutic Agents ◽  
Simultaneous Estimation ◽  
Atorvastatin Calcium ◽  
Ultraviolet Absorbance

Keywords: Simultaneous estimation, combined dosage forms, Atorvastatin, Nateglinide. In the present work, the quantitative estimation of both the drugs in combined dosage forms was carried out. A new, simple, reliable, sensitive, rapid, and economical procedure for simultaneous estimation of atorvastatin calcium and nateglinide in a combined dosage form by UV spectroscopy using the simultaneous equation method was developed. Native ultraviolet absorbance maxima of the two chemotherapeutic agents were used. As both compounds do not interact chemically in methanol, the two wavelengths 246.15 nm for atorvastatin calcium and 206.6 nm for nateglinide were used. Both the drugs obeyed Beer's law in the concentration range (1-10 µg/ml) that was employed in this method. The method developed was validated to determine its linearity (r2=0.996 for atorvastatin and r2=0.997 for nateglinide), precision, reproducibility, and sensitivity. .

scholarly journals Method Development and Validation of Famotidine Oral Suspension by RP-HPLC Method

2020 ◽  
Vol 11 (4) ◽  
pp. 5922-5931
Author(s):  
Prakash chand T ◽  
Elancheziyan K ◽  
Yamini R ◽  
Aysha Jadeera K A ◽  
Vijey Aanandhi M ◽  
...  
Keyword(s):  
Related Compound ◽  
Mobile Phase ◽  
Method Development ◽  
Pharmaceutical Preparations ◽  
Acetate Buffer ◽  
Reverse Phase ◽  
Organic Mixture ◽  
Compound C ◽  
Rp Hplc ◽  
Development And Validation

For perseverance of a simple, fast and selective procedure were developed in drug substance and its pharmaceutical preparations. the proposed project, a successful attempt has been made to develop a simple, accurate, economic and rapid method for the estimation and to validate the method. As a result, a simple, economical, precise and accurate method was developed and validated by Reverse Phase High Performance Liquid Chromatography (RP-HPLC). The main objective for that is to improve the conditions and parameters, which should be followed in the development and validation. developed Reverse phase HPLC technique was done utilizing filtered and degassed pH-6.0 Acetate buffer as a Mobile phase-A and pH-6.0 Acetate buffer and organic mixture in the ratio of 30:70 as a Mobile phase-B. By using waters X-Bridge C18 (150*4.6mm), 3.5µm column separation was achieved. The flow rate and run time was 0.8mL/min and 45minutes. The detection wavelength was 265nm.The average percentage recovery for related compound-C was found to be 94.3%, 95.9%, 96.0% represents the accuracy of the method and for related compound-D was found to be 95.8, 95.4 and 96.4. The %RSD for related compound-C was found to be 5.576 and for related compound-D was found to be 1.588 represents the precision of the method. The correlation coefficient square for , related compound-C and related compound-D was found to be 0.999999, 0.9992 and 0.9991 respectively. Respective parameters met the acceptance criteria, from the results concluded that the developed method was precise and accurate.

scholarly journals NANO FORMULATION ANALYSIS: ANALYTICAL METHOD DEVELOPMENT OF ISONIAZID AND SIMULTANEOUS ESTIMATION OF ANTI-TUBERCULAR DRUGS ISONIAZID AND RIFAMPICIN BY RP-HPLC

2017 ◽  
Vol 10 (5) ◽  
pp. 330 ◽  
Author(s):  
Sushruta S Hakkimane ◽  
Bharath Raja Guru
Keyword(s):  
Liquid Chromatography ◽  
Analytical Method ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Double Emulsion ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Antitubercular Drugs ◽  
Rp Hplc

Objective: The objective of the study was to develop and validate a simple and reproducible reverse phase high pressure liquid chromatography (RPHPLC) method for hydrophilic drug isoniazid (INH) to apply for the analysis of the INH in nanoparticle drug formulations. Furthermore, to estimate simultaneously rifampicin (RIF) and INH in combined form.Methods: Isocratic elution with 10 minutes runtime on a C-18 Luna, 5 μ, 100Å, 150 mm column, methanol, and water as mobile phase with detection wavelength at 268 nm was used. INH nanoformulations were prepared by double emulsion solvent evaporation technique. Quantitative analysis of encapsulated drug was estimated via developed RP-HPLC method. Simultaneous estimation for the two drugs was carried out by gradient elution. All chromatographic separation and estimations were obtained on Shimadzu HPLC system.Results: INH eluted with a short retention time (RT) of 4.06 minutes. Method showed good linearity in the range of concentrations 0.01-100 μg/ml. The limit of detection (LOD) and quantification (LOQ) for INH was 0.03 and 0.12 μg/mL, respectively, and developed method has been successfully applied for the analysis of drugs in nanoparticle formulations. Simultaneous estimation of antitubercular drugs INH and RIF showed two separate peaks within specified runtime.Conclusion: Developed method showed good resolved peaks. Since the RT is short, in a shorter duration more samples could be completed and developed method will be easy for analyzing greater number of samples. Analysis of nanoformulation results have shown that this method is simple, reliable, reproducible, hence can be applied for drug delivery analysis.Keywords: Antitubercular drugs, Reverse phase high performance liquid chromatography, Analytical method development.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR SIMULTANEOUS ESTIMATION OF LAMIVUDINE AND ZIDOVUDINE IN TABLET BY REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2020 ◽  
pp. 73-77
Author(s):  
BHOOMI D PATEL ◽  
MEHTA BHAVYA ◽  
ANKIT B CHAUDHARY
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Rp Hplc

Objective: The objective of the study was to develop and validate reverse-phase high-performance liquid chromatography (RP-HPLC) method and apply method to tablet dosage form. Methods: A simple, rapid, economical, precise, and accurate RP-HPLC method for simultaneous estimation of lamivudine and zidovudine in their combined dosage form has been developed. Results: A RP-HPLC method was developed for the simultaneous estimation of lamivudine and zidovudine. In their combined dosage form has been developed. The separation was achieved by LC-C18 column (150 mm ×4.6 mm, 5 μm) and water: methanol (65:35v/v) as mobile phase, at a flow rate of 0.8 ml/min. Detection was carried out at 272 nm. Retention time of lamivudine and zidovudine was found to be 3.007 min and 4.647, respectively. The method has been validated for linearity, accuracy, and precision. The assay method was found to be linear from 50% to 150% for lamivudine and zidovudine. Conclusion: Developed method was found to be accurate, precise, and rapid for simultaneous estimation of lamivudine and zidovudine in their combined dosage form.

scholarly journals Method Development, Validation and Stability Indicating Studies for Simultaneous Estimation of Anti-Hypertensive Drugs from Pharmaceutical Formulation by RP-HPLC

2020 ◽  
Vol 10 (6) ◽  
pp. 120-132
Author(s):  
V. M. Bhalme ◽  
P. P. Jumade ◽  
Ram D Bawankar ◽  
D. S. Wanjari ◽  
D. R. Mundhada
Keyword(s):  
Mobile Phase ◽  
Room Temperature ◽  
Method Development ◽  
Pharmaceutical Formulation ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Reverse Phase Chromatography ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Degradation Studies

Objective: Method development, validation & stability indicating studies for simultaneous estimation of Anti-Hypertensive drugs, Benidepine (BEN) and Metoprolol (MET) from pharmaceutical formulation by RP-HPLC. Methods: For present work, reverse phase chromatography was selected as its suggested use for ionic and moderate to non-polar compounds. Reverse phase chromatography is simple, suitable, better regarding efficiency, stability, and reproducibility. C18 packed column, a 100 X 2.1mm. ID column of 5.0 μm particle packing, was selected for separation of BEN and MET. Different solvent systems were tried and optimized in combinations as mobile phase. BEN (4 μg/ml) and MET (50 μg/ml) in 15mM ammonium formate-Methanol (15:85 v/v) was developed as it was showing good peak shapes and a significant amount of resolution. The mobile phase was flowed at 1.2 ml/min with detection of BEN analytes at 236 nm and MET analytes at 225 nm respectively. Result: Method development was done. Specificity, linearity, accuracy, precision, robustness, limit of detection and limit of quantitation were used to accomplish validation. The method was found linear from 32.5 – 500 µg.ml-1 for both BEN and MET individually. The percentage recovery of BEN when placed for period of 12 hours was found to 100% in 0.1N/M NaOH at 60˚C and Thermal (60˚C); 12 % degradation in 0.1N/M HCl at 60˚C; Oxidation (3-6% H2O2) at room temperature whereas for MET was 100 % in 0.1N/M NaOH, 0.1N/M HCl at 60˚C, at thermal (60˚C) as well as oxidation by 3-6% H2O2 at room temperature.  Conclusion: Developed analytical method for the simultaneous estimation of Benidipine (BED) and Metoprolol (MET) in both bulk and tablet formulation has obliged the ICH guidelines including, tailing factor (T), separation factors (α), theoretical plates (N), capacity factor (k’), resolution (R) and RSD (%). The validated stress degradation studies under thermal, oxidative, alkali and acid ascertained few degradation products for Benidipine whereas the Metoprolol was unaffected with forced degradation studies. Keywords: Benidipine, Metoprolol, Reverse-Phase High Performance Liquid Chromatography, Stability indicating method.

scholarly journals Analytical Method Development and Validation for the Simultaneous Estimation of Aspirin, Clopidogrel and Rosuvastatin in Pharmaceutical Dosage Form

2019 ◽  
Vol 9 (4-s) ◽  
pp. 432-438
Author(s):  
Pradip Kumar Tiwari ◽  
Amit Jain ◽  
BK Dubey ◽  
GK Pandey ◽  
Suresh Dhakad
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Quantitative Estimation ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Relative Standard

A new, simple, novel, accurate, precise, reliable, rapid and linear reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and fully validated for simultaneous qualitative and quantitative estimation of   Rosuvastatin (ROS), Clopidogrel (CLOP) and Aspirin (ASP) in bulk and pharmaceutical dosage form as per International Conference on Harmonization (ICH) guidelines. In the present work, good chromatographic separation was achieved by isocratic method using a Hypersil BDS C18 column (250 mm ×4.6, 5 μm) and a mobile phase consisting of KH2Po4 buffer pH-6.0: acetonitrile in the ratio 60:40, at a flow rate of 1 ml/min. The effluents obtained were monitored at 242nm with the UV-visible detector. The calibration curves obtained were linear (r2=0.999) over the concentration range of 7.5-22.5μg/ml and 1-3μg/ml for CLOP, ASP and ROS respectively. A run time of 7.0 minutes for each sample made it possible to analyze more than 200 samples per day. The retention time of ASP, CLOP and ROS was found to be 3.103 min, 4,277 min and 5.707 min respectively. The high recovery values (99%-101%) indicate a satisfactory accuracy. The low percent relative standard deviation (% RSD) values in the precision study reveal that the method is precise  therefore the method can be used for routine monitoring of CLOP, ASP and ROS in industry in the assay of bulk drug and dosage form. Keywords: RP-HPLC, Rosuvastatin, Clopidogrel, Aspirin, Method validation, ICH guidelines.

scholarly journals A VALIDATED ANALYTICAL METHOD FOR THE SIMULTANEOUS ESTIMATION OF CYTARABINE AND DAUNORUBICIN IN BULK AND INFUSION FORMULATION BY REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 128-131 ◽  
Author(s):  
PRASANTHI CHENGALVA ◽  
LATHA LAVANYA PEDDAVENGARI ◽  
MADHAVI KUCHANA
Keyword(s):  
High Performance ◽  
Quantitative Estimation ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Reverse Phase ◽  
Column Temperature ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Relative Standard

Objective: The novel liposomal infusion formulation of cytarabine and daunorubicin liposomal infusion is considered as new hope in acute myeloid leukemia treatment. The objective of the present study is to develop and validate a simple, rapid, accurate, precise and sensitive reverse-phase high-performance liquid chromatographic (RP-HPLC) method for the simultaneous estimation of cytarabine and daunorubicin in bulk and infusion formulation. Methods: The chromatographic separation of the drugs was achieved on Denali C18 (250 mm×4.6 mm, 5 μm) in isocratic mode with mobile phase consisting of water (pH was adjusted to 3):acetonitrile in the ratio of 55:45 with a flow rate of 1 ml/min at a detection wavelength of 240 nm using photodiode array (PDA) detector. The column temperature was set at 30°C with 10 μl injection volume. The proposed method was validated as per the International council for Harmonisation (ICH) guidelines. Results: The retention times for cytarabine and daunorubicin were found to be 2.323±0.12 min and 3.140±0.16 min, respectively. Linearity (r2=0.999) was observed over a concentration range of 16.2–97.5 μg/ml for cytarabine and 7.2–43.5 μg/ml for daunorubicin. The percentage relative standard deviation (RSD) for precision studies was found to be 0.2 for both the drugs. Conclusion: A simple, rapid, economic, accurate, and precise RP-HPLC method was developed for simultaneous quantitative estimation of cytarabine and daunorubicin, and the method was validated as per the ICH guidelines. Hence, the method can be employed for the routine analysis of cytarabine and daunorubicin in bulk and infusion formulation.

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