Microwave Mediated Synthesis and Analytical Method Development for the Estimation of Novel 1,4-Dihydropyridines in Bulk by RP-HPLC

Drug Research ◽  
2017 ◽  
Vol 68 (05) ◽  
pp. 296-300
Author(s):  
Anupreet Kaur ◽  
Jaspreet Kaur ◽  
Ranju Bansal
Keyword(s):  
Flow Rate ◽  
Linear Response ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Plate Count ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Standard Solution

AbstractThe present work describes a rapid and green microwave mediated method for the synthesis and a simple and precise isocratic reverse phase HPLC method for the estimation of the biologically significant dihydropyridines. The conventional synthesis of these dihydropyridines has been previously reported from our lab. The analysis of a standard solution (1 mg/ml) was accomplished on a symmetry (4.6 mm I.D x 250 mm) C-18 column using mobile phase acetonitrile:water:triethylamine (TEA) (70:30:0.1 v/v/v) at a flow rate of 0.7 ml/min. Detection was monitored at 354 nm. The retention time for all the compounds was accomplished as less than 10 min. The compounds showed the linear response over the concentration range 10–100 µg/ml. The study is aimed to develop a rapid method for the quantification of these potent molecules. Various parameters like linearity (10–100 µg/ml), USP tailing and plate count were found to be satisfactory. The investigated parameters were studied with the freshly prepared solutions.

scholarly journals RP-HPLC Determination of Raloxifene in Pharmaceuticl Tablets

2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.

A VALIDATED RP-HPLC METHOD FOR THE SIMULTANEOUS ESTIMATION OF PANTOPRAZOLE AND CINITAPRIDE IN A PHARMACEUTICAL FORMULATION

INDIAN DRUGS ◽  
2014 ◽  
Vol 51 (01) ◽  
pp. 27-33
Author(s):  
N. R Dighade ◽  
◽  
S. P. Padmane ◽  
A. V. Kasture
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Capsule Formulation ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Effluent Flow Rate

The study describes a validated stability indicating reverse- phase HPLC method for the simultaneous estimation of pantoprazole and cinitapride in capsule formulation. The proposed RP-HPLC method utilizes an Eclipse XDB C18 Column (150 × 4.6 mm i.d., 5μm), optimum mobile phase consisting of 10 mM phosphate buffer: acetonitrile: THF in the ratio of 64:36:0.5 V/V (pH 3.5) V/V, effluent flow rate 1 mL/min and UV detection wavelength of 266 nm. The selected chromatographic conditions were found to effectively separate pantoprazole and cinitapride with retention time of 7.17 min and 3.56 min, respectively. Linearity for pantoprazole and cinitapride was found in the range of 2-30 μg/mL and 0.15- 2.28 μg/mL, respectively. The developed method was statistically validated for the linearity, accuracy, precision, robustness, ruggedness and specificity. The proposed method was found to be simple, accurate, precise, economical and specific. Therefore, it can be used for simultaneous analysis of these drugs in capsule formulation.

scholarly journals APPLICATION OF VALIDATED RP-HPLC METHOD FOR THE DETERMINATION OF ARMODAFINIL IN BULK AND FORMULATION

2017 ◽  
pp. 158-161
Author(s):  
Devi Ramesh ◽  
Mohammad Habibuddin
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Isocratic Mode

Objective: The objective of the present study is to develop and validate a simple, rapid, sensitive reverse phase HPLC method for the determination of Armodafinil present in bulk and its pharmaceutical formulations.Methods: The chromatographic separation was achieved by using Hypersil ODS C-18 (150 x 4.6 mm, 5µ) in an isocratic mode with mobile phase methanol: phosphate buffer 3.0 (60:40 %v/v) was used. The flow rate was 1 ml/min and effluent was monitored at 225 nm. The method was validated for validation parameters i.e. linearity, accuracy, precision and robustness according to ICH guidelines.Results: The retention time of Armodafinil was 4.2 min and the linearity range of the method was 500-20000ng/ml with regression (r2) coefficient 0.9998. The method was validated for precision, accuracy, robustness and which were found to be within the acceptable limits according to the ICH guidelines. Also, the method was successfully applied for the estimation of Armodafinil in the marketed formulation of Nuvigil and the recovery was found to be>98%.Conclusion: The developed method possess good selectivity, specificity, there is no interference found in the blank at a retention time of ARM and good correlation between the peak area and concentration of the drugs under prescribed conditions. Hence, the method can be applied for routine analysis of Armodafinil. 

scholarly journals Method Development for 4-Hydroxy-2-Methyl-N- (5-Methyl-2-Thiazolyl)-2H-1,2-Benzothiazine-3-Carboxamide-1,1-Dioxide by Reverse Phase HPLC: New Analytical Technique

2019 ◽  
pp. 1-10
Author(s):  
Husnul Maab ◽  
Hammad Yousaf ◽  
Syed Saeed ul Hassan ◽  
Umar Farooq
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Raw Material ◽  
New Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Analytical Technique ◽  
Peak Areas ◽  
Standard Solution ◽  
Study Development

Purpose: In this study, development of a new analytical method for the evaluation of 4-Hydroxy-2-methyl-N-(5-methyl-2-thiazolyl)-2H-1,2-benzothiazine-3-carboxamide-1,1-dioxide (Meloxicam) by reverse phase HPLC was carried out. The basic aim of this research was to develop and validate a simple, precise, accurate and sensitive method for qualitative and quantitative analysis of Meloxicam in pharmaceutical raw material and its dosage forms. The existing reported method (BP) for the analysis of Meloxicam is potentiometric method which is an old, lengthy and tedious method. Methods: In the new method of reverse phase HPLC, C18 column was used while the mobile phase was acetonitrile and methanol (70:30). The flow rate of mobile phase was 0.6 ml/min and retention time was found to be 1.5min. Separately equal volume of standard solution and sample solutions in HPLC vials were injected in auto sampler compartment of HPLC in six replicates. Chromatogram and peak areas of Meloxicam in standard and sample solutions of different concentrations were recorded. Results: This method was later validated in different ways by which the calibration curve proved to be linear with linearity coefficient of 0.999 over the range of 100 to 600ppm. The precision was equivalent to 0.0003%. The LOD and LOQ were 0.0003ug/ml and 0.001ug/ml respectively. The system also showed accuracy over the range of 95 to 99%. Conclusion: Hence, this method proved to be an alternative to the existing reported method of potentiometric titration because the new method showed accuracy, reproducibility and sensitivity.

scholarly journals RP-HPLC Method Development and Validation for the Estimation of Lansoprazole in Presence of Related Substances by QbD Approach

2021 ◽  
pp. 138-150
Author(s):  
Sachin B. Gholve ◽  
Jaiprakash N. Sangshetti ◽  
Omprakash G. Bhusnure ◽  
Ram S. Sakhare ◽  
Pratap H. Bhosale ◽  
...  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Drug Substance ◽  
Gastric Ulcers ◽  
Mobile Phase Flow Rate ◽  
Column Temperature ◽  
Rp Hplc

A rapid specific RP-HPLC method has been developed for the determination of Lansoprazole impurities in the drug substance. The control of pharmaceutical impurities is currently a critical issue in the pharmaceutical industry. The International Council for Harmonization (ICH) has formulated a workable guideline regarding the control of impurities. The objective of the recent study was to develop and validate a HPLC method for the quantitative determination of process-related impurities of Lansoprazole in pharmaceutical drug substance. Lansoprazole, 2-[[[3-methyl-4-(2,2,2-trifluoroethoxy)-2-pyridinyl] methyl]-sulfinyl]- 1H-benzimidazole is an proton pump inhibitor used in the management of gastric ulcers. Chromatographic identification of the impurities was carried out by response surface methodology, applying a three-level Box Behnken design with three center points. Three factors selected were a mobile phase, flow rate, column temperature. Evaluation of the main factor, their interaction, and the quadric effect on peak resolution were done on Waters Symmetry C8, 250 x 4.6mm, 5µm column is used for the development of the method. The mobile phase consists of buffer and acetonitrile. The flow rate of the mobile phase was 1.0 ml/min with gradient elution. The column temperature is ambient and the detection wavelength is 235 nm. The injection volume was 10 µL. The method was validated as per ICH guidelines for linearity in the range of 50-150 µg/ml and the LOD & LOQ values obtained were 0.437×10-4 and 0.1325×10-3 µg/ml respectively which specifies the method's sensitivity. The proposed method was successfully used to determine the Lansoprazole impurities in drug substances.

scholarly journals Reverse-phase High-Performance Liquid Chromatography Method Development and Validation for Estimation of Glimepiride in Bulk and Tablet Dosage Form

2020 ◽  
Vol 11 (02) ◽  
pp. 296-302
Author(s):  
Aseem Kumar ◽  
Anil Kumar Sharma ◽  
Rohit Dutt
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Development And Validation

The present work demonstrates a simple, rapid, precise, specific, and sensitive reverse-phase high-performance liquid chromatography (RP-HPLC) method for analyzing glimepiride in pure and tablet forms. The present method was developed using a C18 column 150 × 4.6 mm, with 5 μm, and packing L1 maintained at a temperature of 30°C. The mobile phase was prepared by dissolving 0.5 gram of monobasic sodium phosphate in 500 mL of distilled water, pH of the solution adjusted to 2.1 to 2.7 with 10% phosphoric acid, and added 500 mL of acetonitrile. The mobile phase was pumped in the highperformance liquid chromatography (HPLC) system at a flow rate of 1 mL/min, and separation was carried out at 228 nm, using an ultraviolet (UV) detector. The chromatographic separation was achieved with peak retention time (RT) at about 9.30 minutes, and the method was found to be linear over a concentration range of 40 to 140 μg/mL. The specificity of the method represented no interference of the excipients during the analysis, and stability testing after 24 hours also showed that the method is suitable and specific. The accuracy was between 99.93 to 99.96%, with limit of detection (LOD) and limit of quantitation (LOQ) being 0.354 μg/mL, 1.18 μg/mL, respectively. Satisfactory results were found for precision and robustness parameters during the development and validation stage for the analytical method. The proposed method was also adopted for the analysis of glimepiride tablets to improve the overall quality control. Using this method, symmetric peak shape was obtained with reasonable retention time. The retention time of glimepiride for six repetitions is 9.3 ± 0.1 minutes; the run time is 21 minutes. The proposed RP-HPLC method is a modification of the United States Pharmacopeia (USP) method, and it was found to be valid for glimepiride within concentration ranges 40 to 140 μg/mL, using C18 analytical columns, and isocratic elution with UV detection, and at 1 mL/min of flow rate.

scholarly journals Method Development and Validation of Fludrocortisone Acetate Tablets by Reverse Phase HPLC Method

2020 ◽  
Vol 11 (4) ◽  
pp. 6826-6833
Author(s):  
Vijey Aanandhi M ◽  
Elancheziyan K ◽  
Yamini R ◽  
Prakash Chand T ◽  
Aysha Jadeera K A ◽  
...  
Keyword(s):  
Phosphate Buffer ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Hplc Technique ◽  
Fludrocortisone Acetate ◽  
Development And Validation

The purpose or intent of this current study was to establish a fast and sensitive HPLC technique for the perseverance of Fludrocortisone acetate and utilizing best frequently used HPLC technique. This method had been validated as per the ICH requirements  to assure that the method consistently meets the predetermined specifications and quality attributes.Utilizing filtered and degassed pH 3.0 Phosphate buffer and Acetonitrile in the ratio 90:10 as a Mobile phase-A and pH 3.0 Phosphate buffer and Acetonitrile in the ratio 65:35 as a Mobile phase-B the established RP-HPLC technique was done. The separation was achieved by using Waters, X-Bridge Shield RP18, (150 X 4.6-mm), 3.5-µm column. Run time and Flow rate was set 45minutes and 1.2mL/min. Injection volume 100µL and wavelength was set 240nm.The correlation coefficient square for fludrocortisones acetate and Fludrocortisone Impurity was found to be 0.9991 and 0.99997. The SD and %RSD for Fludrocortisone Impurity was found to be 0.02 and 1.48 represents method precision. Following validated parameters lies within the limit. Hence, the developed method was precise, simple, fast and accurate.

scholarly journals Estimation of Ziprasidone Hydrochloride Monohydrate in Bulk and Capsules by Reverse Phase HPLC

2006 ◽  
Vol 3 (3) ◽  
pp. 169-172 ◽  
Author(s):  
B. Sudha Rani ◽  
P. Venkata Reddy
Keyword(s):  
Flow Rate ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Forms ◽  
Hydrochloride Monohydrate

A reverse phase HPLC method is described for the determination of Ziprasidone HCl mono hydrate in bulk and pharmaceutical dosage forms. Chromatography was carried out on an ODS C18 column using a mixture of methanol and phosphate buffer (55:45v/v) as the mobile phase at a flow rate of 1mL/min. Detection was carried out at 314nm. The retension time of the drug was 4.522 min. The method produced linear responses in the concentration range of 0.5-30 μg /mL of Ziprasidone HCl mono hydrate.The method was found to be applicable for determination of the drug in capsules.

RP-HPLC Method for Quantification of Etelcalcetide in Bulk and Parentral Dosage Form

2021 ◽  
pp. 5521-5526
Author(s):  
Krishna Kishore Adireddy ◽  
Srinivasa Rao Baratam ◽  
Nagarjuna Hari Pratap S.
Keyword(s):  
Flow Rate ◽  
Linear Response ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Solution Stability ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Controller

A simple, rapid, accurate and precise RP-HPLC method was developed and validated for the determination of Etelcalcetide in bulk and parentral dosage form. Quantification of the drug was achieved on Shimadzu HPLC comprising of LC- 20 AD binary gradient pump, a variable wavelength programmable SPD-20A detector and SCL system controller. C18G column (250 mm x 4.6 mm, 5 μ) as stationary phase with mobile phase consisting of acetonitrile: methanol :water in the ratio of 25: 45 :30 v/v. The method showed a good linear response in the concentration range of 3.75-22.5 μg/ml with correlation coefficient of 0.9999. The flow rate was maintained at 1.0 ml/min and effluents were monitored at 238 nm. The retention time of etelcalcetide was 6.201 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, solution stability, selectivity and sensitivity. The results obtained in the study were within the limits of ICH guidelines and hence this method can be used for the determination of etelcalcetide in bulk and parentral dosage form.

Development, Validation and Application of HPLC Method for Metformin in Rabbit Plasma

2019 ◽  
Vol 15 (6) ◽  
pp. 574-579
Author(s):  
Muhammad Ubaid ◽  
Mahmood Ahmad ◽  
Farhan Ahmad Khan ◽  
Ghulam Murtaza
Keyword(s):  
Flow Rate ◽  
Present Method ◽  
Mobile Phase ◽  
Hplc Method ◽  
Plasma Samples ◽  
Rabbit Plasma ◽  
Uv Detector ◽  
Reverse Phase ◽  
T Values ◽  
Pharmacokinetic Evaluation

Objective:This study was aimed at conducting a pharmacokinetic evaluation of metformin in rabbit plasma samples using rapid and sensitive HPLC method and UV detection.Methods:Acetonitrile was used for protein precipitation in the preparation of plasma samples. Reverse phase chromatography technique with silica gel column (250 mm × 4.6 mm, 5 μm) at 30°was used for the separation purpose. Methanol and phosphate buffer (pH 3.2) mixture was used as a mobile phase with flow rate 0.8 ml/min. The wavelength of UV detector was adjusted at 240 nm.Results:The calibration curve was linear in a range of 0.1-1 µg/ml with R² = 0.9982. The precision (RSD, %) values were less than 2%, whereas, accuracy of method was higher than 92.37 %. The percentage recovery values ranged between 90.14 % and 94.97 %. LOD and LOQ values were 25 ng/ml and 60 ng/ml, respectively. Cmax and AUC0-t values were found to be 1154.67 ± 243.37 ng/ml and 7281.83 ± 210.84 ng/ml.h, respectively after treating rabbits with a formulation containing 250 mg metformin.Conclusion:Based on the above findings, it can be concluded that present method is simple, precise, rapid, accurate and specific and thus, can be efficiently used for the pharmacokinetic study of metformin.

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