scholarly journals SIMPLE AND RAPID HPLC METHOD FOR SIMULTANEOUS QUANTIFICATION OF LEVODOPA AND CARBIDOPA IN A FAST DISINTEGRATING TABLET FORMULATION

2019 ◽  
pp. 200-205
Author(s):  
Shohreh Alipour ◽  
MAHSA ASEF ◽  
FATEMEH AHMADI
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Wet Granulation ◽  
Dissolution Profile ◽  
Limit Of Quantification ◽  
Disintegration Time ◽  
Simultaneous Quantification ◽  
Rp Hplc ◽  
First Choice ◽  
Fast Disintegrating Tablets

Objective: Fast disintegrating tablets (FDTs) are found helpful in dysphagia (difficulty in swallowing) especially in Parkinson patients. Levodopa is still the first choice in Parkinson disease treatment and is co-administered by carbidopa for better efficacy. Methods: In the present study, a rapid and simple isocratic Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) method was developed and validated for simultaneous quantification of levodopa and carbidopa in optimized Fast Disintegrating Tablets (FDTs). The linearity, precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ) of the method were determined. FDTs were prepared using direct compression, dry and wet granulation and were optimized for faster disintegration time. Tablets thickness, weight, hardness, friability, drug content and dissolution profile were also evaluated. Results: A RP-HPLC system with C18 column and mobile phase 90:10 (v/v) phosphate buffer: methanol was used. The method linearity was found to be within the concentration range of 3.125-50 μg/ml for levodopa, and 3.125-25 μg/ml for carbidopa. The intra and inter-day precision and accuracy were acceptable. LOD and LOQ of levodopa-carbidopa were 0.2-0.8 μg/ml and 0.5-2.4 μg/ml, respectively. The total chromatographic run time was 5 min. The optimized FDTs hardness was 3.81±0.4 and tablets were disintegrated within 30 sec. Levodopa and carbidopa were dissolved in dissolution media within 5 min. Conclusion: Results indicated that this method was suitable for simultaneous quantification of levodopa and carbidopa in the presence of different ingredients of a pharmaceutical solid dosage form. Therefore, this method could be applied in pharmaceutical quality control for rapid quantification of structurally similar substances with different physicochemical properties.

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

RP-HPLC Method Development and Validation for the Estimation of Sacubitril and Valsartan in Pharmaceutical Dosage Form

2021 ◽  
pp. 5797-5802
Author(s):  
G.M. Kadam ◽  
A.L. Puyad ◽  
T.M. Kalyankar
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Content Uniformity ◽  
Phase Detection ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Hplc Method Development

A new, economical, simple, accurate, and precise RP-HPLC method was developed for simultaneous assay and content uniformity determination of Sacubitril and Valsartan in bulk and pharmaceutical dosage form. The separation of Sacubitril and Valsartan was achieved within 6 minutes on Phenomenex Luna C18 250 mm x 4.6mm and 5µm Particle Size, column using Acetonitrile: Methanol: Water (30:55:15% v/v/v) as the mobile phase. Detection was carried out at 250 nm wavelength. The retention time of Sacubitril and Valsartan was found to be 2.361 and 3.304 min, respectively. The validation of the developed method was performed in terms of specificity, accuracy, precision, linearity, the limit of detection, the limit of quantification as mentioned in International Conference on Harmonization (ICH) guidelines. The method showed adequate sensitivity concerning linearity, accuracy, and precision over the range 12-36 μg/ml and 13-39 μg/ml for Sacubitril and Valsartan, respectively. The percentage recoveries obtained for Sacubitril and Valsartan were found to be in the range of 98.00 – 102.00 %. The proposed method is suitable for use in quality-control laboratories for quantitative analysis.

scholarly journals LC-MS characterization of acid degradation products of metoclopramide: Development and validation of a stability-indicating RP-HPLC method

2020 ◽  
Vol 11 (1) ◽  
pp. 781-789
Author(s):  
Sriram Valavala ◽  
Nareshvarma Seelam ◽  
Subbaiah Tondepu ◽  
Suresh Kandagatla
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Hplc Technique

The present study aims to develop a simple, accurate and specific stability-indicating RP-HPLC technique for the analysis of metoclopramide in the presence of its stress degradation products and characterization of degradation compounds by LC-MS/MS analysis. As per ICH Q1A-R2 guidelines, the drug was exposed to acid hydrolytic stress condition. Three degradation products were formed for MCP in acid hydrolysis. The liquid chromatography was processed on a Luna C18-(2) 100A,250×4.6mm 5micron column using an isocratic mobile phase consisting of 0.1% formic acid in water-acetonitrile (20:80, v/v) by adjusting the mobile phase at 1 ml/min flow rate with wavelength detection at 273 nm. The developed procedure was applied to LC-MS/MS (liquid chromatography-tandem mass spectrometry) for the characterization of all the degradant components. Total new three degradation compounds were recognized and identified by LC-MS/MS. The developed RP-HPLC technique was validated as per the ICH Q2-R1 guidelines. Limit of detection and limit of quantification values of MCP were evaluated from the linearity graph and were found to be 5.23 µg/ml and 17.44 µg/ml. Accuracy study was established at 80.0, 100.0 and 120.0 µg/ml concentration levels and the findings were found in the range of 98.4% - 101.8%. The linearity of the technique was assessed over the drug concentration range of 50.0 µg/ml to 250.0 µg/ml and the regression equation, slope and correlation coefficient values were found to be y = 10618x + 1623.2, 10618 and 0.9996 respectively. The developed technique was uninterruptedly applied for the quantification of metoclopramide inactive pharmaceuticals.

METHOD DEVELOPMENT AND VALIDATION OF IXAZOMIB DRUG BY RP-HPLC IN BULK AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (01) ◽  
pp. 28-34
Author(s):  
Yarasani Prashanthi ◽  
◽  
Faheem Ahmed ◽  
Tentu Nageswara Rao ◽  
Botsa Parvatamma ◽  
...  
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Temperature Detector ◽  
Theoretical Plates

A novel approach was used for develop and validate a rapid, accurate, and an isocratic RP-HPLC method with PDA detector for the estimation of ixazomib drug in pharmaceutical dosage forms. Ixazomib was seperated using Agilent 4.6*150 mm, 5μm analytical column, a Waters HPLC system (USA) and a mobile phase consisting of water and acetonitrile in the ratio of 40:60 V/V. The flow rate was set to 0.7 mL/min with 10µL injection volume. The column was maintained at ambient temperature, detector was set at wavelength of 274 nm. The retention time of ixazomib was found to be 2.17 min. The system suitability parameters for ixazomib such as theoretical plates and tailing factor were found to be 4146. Linearity was established for ixazomib such as theoretical plates and telling factor were found to be 4146. Linearilty was established for ixazomib in the range of 50-250 µg/ml concentration levels with correlation coefficients (r2) of 0.999. The intra-and inter-day precision % RSD values were found to be 0.47 and 0.31, respectively. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 2.03 and 6.17 µg/mL respectively. The method was validated for all of the above parameters according to the International Conference on Harmonization (ICH) guidelines. This method can be used for estimation and analysis of ixazomib drug in active pharmaceutical ingredients and pharmaceuticals.

scholarly journals NOVEL RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF TELMISARTAN AND NEBIVOLOL HCL IN PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 (9) ◽  
pp. 431 ◽  
Author(s):  
Heena Ar Shaikh ◽  
Vandana Jain
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Hplc Method Development

Objective: A simple, accurate, precise, robust reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the estimation of telmisartan and nebivolol hydrochloride (HCl) simultaneously in its combined dosage form.Methods: The compounds were well resolved in an isocratic method using the mobile phase composition of acetonitrile: Buffer (potassium dihydrogen orthophosphate pH adjusted 3.1 with orthophosphoric acid) in a ratio of 40:60 v/v at a flow rate of 1.2 ml/min using C18 Shim-pack (150 mm × 4.6 mm, 5 μ) column. The detection was carried out at 280 nm.Results: The retention time of telmisartan and nebivolol HCl was 4.8 min and 6.5 min, respectively. The developed method was validated by evaluating various validation parameters such as linearity, precision, accuracy, robustness, specificity, limit of detection, and limit of quantification according to the international council for harmonization guidelines. The standard calibration curve was obtained in the concentration range of 24–56 μg/ml for telmisartan and 3–7 μg/ml for nebivolol HCl. The overall average % recovery was found out to be 100.35 for telmisartan and 98.84 for nebivolol HCl.Conclusion: Statistical analysis of the data showed that the method is reproducible and selective for the estimation of telmisartan and nebivolol HCl. The proposed method could be used for analysis of telmisartan and nebivolol HCl in their dosage form.

scholarly journals A Validated RP-HPLC Method for Estimation of Related Compounds in Hydroxy Naproxen

2020 ◽  
Vol 32 (5) ◽  
pp. 1158-1164
Author(s):  
L. Vaikunta Rao ◽  
K. Tirumala Rao ◽  
V.V. Krishna Mohan Kandepi
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Assay Method ◽  
Array Detector ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Related Substance ◽  
Mobile Phase Flow Rate ◽  
Rp Hplc ◽  
Related Compounds

A simple, linear gradient liquid chromatographic method (RP-HPLC) is proposed for the simultaneous estimation of related compounds in hydroxy naproxen samples. Chromatographic separation was achieved on Zorbax SB C8 (150 × 4.6) mm, 3.5 μm particle size RRLC short column and eluent A used as 0.1% v/v trifluoroacetic acid in water and eluent B used as acetonitrile using Agilent RRLC (UHPLC) system. The mobile phase flow rate was 1.0 mL/min and the eluted compounds were monitored at 235 nm for related substance method and assay method. The excellent resolution was obtained between hydroxy naproxen and its related compounds, which were eluted within 25 min. The performance of the method was validated with respect to ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision and robustness. The correlation coefficient(r) was > 0.995 for both the methods from linearity data and percentage of recovery is 98.0 to 102.0 for assay method and 80.0 to 120.0% for related substance method. Sensitivity of the method was found be less than 0.5 μg/mL. Peak homogeneity data for naproxen in the chromatograms from the selectivity solution obtained by use of the photodiode array detector demonstrated the specificity of the method for analysis of hydroxy naproxen in presence of the related compounds

scholarly journals Development and Validation of an RP-HPLC Method for CB13 Evaluation in Several PLGA Nanoparticle Systems

2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
Author(s):  
J. Álvarez-Fuentes ◽  
L. Martín-Banderas ◽  
I. Muñoz-Rubio ◽  
M. A. Holgado ◽  
M. Fernández-Arévalo
Keyword(s):  
Size Distribution ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Plga Nanoparticles ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Rp Hplc

A simple, fast, and reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed and validated for determining of a cannabinoid derivate, which displays potent antihyperalgesic activity, 1-naphthalenyl[4-(pentyloxy)-1-naphthalenyl]methanone (CB13) into PLGA nanoparticles. Separation was achieved in a C18 column using a mobile phase consisting of two solvents: solvent A, consisting of acetonitrile : water : acetic acid (75 : 23.7 : 1.3 v/v), and solvent B, consisting of acetonitrile. An isocratic method (70 : 30 v/v), with a flow rate of 1.000 mL/min, and a diode array detector were used. The developed method was precise, accurate, and linear over the concentration range of analysis with a limit of detection and a limit of quantification of 0.5 and 1.25 μg/mL, respectively. The developed method was applied to the analysis of CB13 in nanoparticles samples obtained by three different procedures (SEV, FF, and NPP) in terms of encapsulation efficiency and drug release. Nanoparticles size and size distribution were also evaluated founding that NPP method presented the most lowest particle sizes with narrow-size distribution (≈320 nm) and slightly negative zeta potential (≈−25 mV) which presumes a suitable procedure for the synthesis of PLGA-CB13 nanoparticles for oral administration.

scholarly journals RP-HPLC Method Development and Validation for the Estimation of Mirabegron in Bulk and Dosage Form

2020 ◽  
Vol 10 (1) ◽  
pp. 31-38
Author(s):  
Rahul Suryawanshi ◽  
Siddiqua Shaikh ◽  
Snehal Patil
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Hplc Method Development ◽  
Tablet Dosage

A new, simple, precise, accurate and reproducible Reverse Phase High Performance Liquid Chromatography (RP-HPLC) method for Simultaneous estimation of bulk and pharmaceutical formulations. Separation of Mirabegron was successfully achieve , C18, 250X4.6mm, 5µm or equivalent in an isocratic mode utilizing methanol water (70:30) at pH 5.0 Adjusted to OPA at a flow rate of 1.0ml/min and eluate was monitored at 243nm, with a retention time of 2.584 minutes for Mirabegron. The method was validated and the response was found to be linear in the drug concentration range of 50µg/ml to150 µg/ml for Mirabegron. The values of the correlation coefficient were found to 0.999for Mirabegron. The Limit of Detection(LOD) and Limit of Quantification (LOQ) for Mirabegron were found to be 0.149 and 0.498 respectively. This method was found to be good percentage recovery were found to be 99 indicates that the proposed method is highly accurate. The specificity of the method shows good correlation between retention times of standard with the sample so, the method specifically determines the analyte in the sample without interference from excipients of tablet dosage forms. The method was extensively validated according to International Council for Harmonisation(ICH) guidelines for Linearity, Accuracy, Precision, Specificity and

scholarly journals Spectrophotometric and RP-HPLC Methods for Determining Cefotaxime Sodium in Pharmaceutical Preparations

2020 ◽  
Vol 32 (6) ◽  
pp. 1314-1320
Author(s):  
Lamya A. Sarsam ◽  
Salim A. Mohammed ◽  
Sahar A. Fathe
Keyword(s):  
Limit Of Detection ◽  
Phosphate Buffer Solution ◽  
Pharmaceutical Preparations ◽  
Molar Absorptivity ◽  
Hplc Method ◽  
Buffer Solution ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard

A rapid, simple and sensitive spectrophotometric and RP-HPLC methods have been developed for the quantitative determination of cefotaxime-Na in both pure and dosage forms. The spectrophotometric method was based on diazotization of cefotaxime-Na and then coupling with 8-hydroxyquinoline in an alkaline medium. The resulting azo dye exhibited maximum absorption at 551 nm with a molar absorptivity of 0.597 × 104 L mol-1 cm-1. Beer′s law was obeyed over the range 10-700 μg/25 mL (i.e. 0.4-28.0 ppm) with an excellent determination coefficient (R2 = 0.9993). The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.0194 and 0.3765 μg mL-1, respectively. The recoveries were obtained in the range 97.3-102.5% and the relative standard deviation (RSD) was better than ± 1.56. The HPLC method has been developed for the determination of cefotaxime-Na. The analysis were carried out on a C18 column and a mobile phase composed of acetonitrile and phosphate buffer solution (0.024M KH2PO4 and 0.01M H3PO4) at pH 3.5 in the ratio of 60:40 (v:v), with a flow rate of 1.0 mL min-1 and UV detection at 258 nm. The proposed method showed good linearity (in a range of concentration 1.0-200 μg mL-1. The recovery percent and a relative standard deviations were found in the range 96 to 104.8% and ± 0.017 to ± 0.031%, respectively. Both methods were applied successfully to the assay of cefotaxime-Na in commercial injection preparations.

RP-HPLC Assay for Estimation of Pitavastatin in Bulk and Pharmaceutical Dosage Forms

2014 ◽  
Vol 7 (1) ◽  
pp. 2346-2349
Author(s):  
K Tirumala ◽  
CH.V.S Gautam ◽  
J Gangadhar ◽  
M Jayajeevitha ◽  
Vanitha Prakash K
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Dosage Forms ◽  
Hplc Method ◽  
Detector Response ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Bulk Drug

Reverse phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for the estimation of pitavastatin in tablet dosage form. A Phenomenex Luna C18, 150×4.6 mm i.d, 5 µm particle size with mobile phase consisting of buffer 0.01M potassium dihydrogen ortho phosphate pH (3.75) adjusted with dilute orthophosphoric and acetonitrile in the ratio of 20:80 v/v was used. The flow rate was 1.2 mL/min and eluents were monitored at 248 nm. The retention time was 4.1min. The detector response was linear in the concentration of 25-150 µg/mL, with the regression coefficient of 0.9998. Quantification was done by calculating area of the peak and the limit of detection and limit of quantification were 1.9 µg/mL and 5.7 µg/mL respectively. The percentage assay of pitavastatin was 101.1%. The results of study showed that the proposed RP-HPLC method is simple, rapid, precise and accurate which is useful for the routine determination of pitavastatin in bulk drug and in its pharmaceutical dosage forms.

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