scholarly journals Development and Validation of LC Method for the Determination of Famciclovir in Pharmaceutical Formulation Using an Experimental Design

2008 ◽  
Vol 5 (1) ◽  
pp. 58-67 ◽  
Author(s):  
Srinivas Vishnumulaka ◽  
Narasimha Rao Medicherla ◽  
Allam Appa Rao ◽  
G. Edela Srinubabu
Keyword(s):  
Experimental Design ◽  
Flow Rate ◽  
Mobile Phase ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Internal Standard Method ◽  
Intermediate Precision ◽  
Mobile Phase Flow Rate ◽  
Development And Validation

A rapid and sensitive RP-HPLC method with UV detection (242 nm) for routine analysis of famciclovir in pharmaceutical formulations was developed. Chromatography was performed with mobile phase containing a mixture of methanol and phosphate buffer (50:50,v/v) with flow rate 1.0 mL min−1. Quantitation was accomplished with internal standard method. The procedure was validated for linearity (correlation coefficient =0.9999), accuracy, robustness and intermediate precision. Experimental design was used for validation of robustness and intermediate precision. To test robustness, three factors were considered; percentage v/v of methanol in mobile phase, flow rate and pH; flow rate, the percentage of organic modifier and pH have considerable important effect on the response. For intermediate precision measure the variables considered were: analyst, equipment and number of days. The RSD value (0.86%,n=24) indicated an acceptable precision of the analytical method. The proposed method was simple, sensitive, precise, accurate and quick and useful for routine quality control.

scholarly journals DEVELOPMENT AND VALIDATION OF A SIMPLE HPLC METHOD FOR ESTIMATION OF MYCOPHENOLATE MOFETIL IN MICROEMULSION FORMULATION

2020 ◽  
pp. 16-20
Author(s):  
PALAKDEEP KAUR ◽  
MOHIT KUMAR ◽  
UTTAM KUMAR MANDAL
Keyword(s):  
Mycophenolate Mofetil ◽  
Flow Rate ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Mobile Phase Flow Rate ◽  
Boundary Limit ◽  
Development And Validation

Objective: The present study deals with the development, validation and application of a simple, precise and accurate HPLC method for the determination of mycophenolate mofetil in pharmaceutical formulations and microemulsions. Methods: In this method, a simple isocratic mobile phase composition of methanol and water (75:25 v/v) pumped at 1 ml/minute flow rate through Phenomenex C18 column (dimension: 250 4.6 mm and 5 µm particle size) was used. Injection volume was 20 µl and analysis of mycophenolate mofetil was carried out at 250 nm. Results: The coefficient of regression was found to be 0.9996, indicating the linearity of the developed method within a range of 0.1 to 10 µg/ml. The limit of detection (LOD) and the limit of quantization (LOQ) were found to be 3.660ng/ml and 11.091ng/ml, respectively. The results showed that % deviation for change in compositions of the mobile phase, flow rate and temperature was within a range of-5.51 to 10.99%,-3.70 to 8.80% and-5.29 to 10.90%, respectively. The method seemed sensitive to change of temperature (±5 ○C) and methanol composition (±2%) as the results were at the boundary limit of 10% deviation. Conclusion: A simple, precise and accurate HPLC method for the determination of drug content from microemulsion has been developed and validated in accordance with ICH guidelines.

scholarly journals Development and Validation of an HPLC Method for the Determination of the macrolide antibiotic Clarithromycin using Evaporative Light Scattering Detector in raw materials and Pharmaceutical Formulations

2017 ◽  
Vol 6 (4) ◽  
pp. 133-141 ◽  
Author(s):  
Zampia Tzouganaki ◽  
Michael Koupparis
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Gas Flow ◽  
Raw Materials ◽  
Pharmaceutical Formulations ◽  
Reversed Phase ◽  
Hplc Method ◽  
Ich Guidelines ◽  
Development And Validation

In this work, ELS-Detector has been used for the development of an HPLC method for the determination of clarithromycin in pharmaceutical formulations (tablets and pediatric suspension). Isocratic reversed phase HPLC approach has been developed using a C-18 column (Waters Spherisorb 5 μm ODS2, 4.6x250 mm) and a mobile phase consisting of acetonitrile / aqueous trifluoroacetic acid as pairing reagent. Experimental parameters (temperature of heated drift tube, flow rate of mobile phase, gas flow rate, mobile phase composition) were optimized. Clarithromycin’ s stability was thoroughly examined in different solvent systems. Using the optimized conditions the working range was 5-100 μg/mL (upper limit can be increased considerably), with a detection limit of 4.5 μg/mL (6x10-6 M). The method was validated as per ICH guidelines. The retention time was 4.7 min. The method was successfully applied for the content assay of clarithromycin formulations.

SIMULTANEOUS ESTIMATION OF CURCUMIN AND GEFITINIB IN BULK AND TISSUE SAMPLES (PLASMA AND BRAIN HOMOGENATE) BY RP-HPLC: APPLICATION TO A DISTRIBUTION STUDY

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 59-68
Author(s):  
H Mahajan ◽  
S Savale ◽  
P Nerkar ◽  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Internal Standard ◽  
Brain Homogenate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Bulk Analysis ◽  
Experimental Conditions ◽  
Rp Hplc

The present study was aimed at developing a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) method for simultaneous determination of curcumin (CRM) and gefitinib (GFT) in bulk, plasma and brain homogenate. hydrochlorothiazide was used as an internal standard (IS). A new simple, rapid, selective, precise and accurate RP-HPLC method has been developed. The separation was achieved by using C-18 column (Qualisil BDS C18, 250 mm x 4.6 mm I.D.) coupled with a guard column of silica, mobile phase consisted of acetonitrile: water with 0.1% formic acid (30:70 v/v). The flow rate was 0.2 ml/min and the drug was detected using PDA detector at the wavelength of 242 nm. The experimental conditions, including the diluting solvent, mobile phase composition, column saturation and flow rate, were optimised to provide high-resolution and reproducible peaks. The method was developed and tested for linearity range of 10-60 μg/mL for bulk analysis and 200-800 ng/mL for plasma and brain homogenate. The developed method was validated as per ICH guidelines, in terms of linearity, application of the proposed method to bulk sample, recovery, precision, repeatability, ruggedness, sensitivity (LOD and LOQ) and robustness and stability study (short and long-term stabilities, freeze/thaw stability, post-preparative). The low value of % RSD showed that the method was precise within the acceptance limit of 2%. The developed method was successfully applied for the analysis of the drug in bulk as well as various marketed formulation and drug in plasma and brain distribution studies.

scholarly journals Reversed phase HPLC for strontium ranelate: Method development and validation applying experimental design

2018 ◽  
Vol 68 (2) ◽  
pp. 171-183
Author(s):  
Béla Kovács ◽  
Lajos Kristóf Kántor ◽  
Mircea Dumitru Croitoru ◽  
Éva Katalin Kelemen ◽  
Mona Obreja ◽  
...  
Keyword(s):  
Experimental Design ◽  
Strontium Ranelate ◽  
Method Development ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Reversed Phase ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Limit Of Quantitation ◽  
Development And Validation

Abstract A reverse-phase HPLC (RP-HPLC) method was developed for strontium ranelate using a full factorial, screening experimental design. The analytical procedure was validated according to international guidelines for linearity, selectivity, sensitivity, accuracy and precision. A separate experimental design was used to demonstrate the robustness of the method. Strontium ranelate was eluted at 4.4 minutes and showed no interference with the excipients used in the formulation, at 321 nm. The method is linear in the range of 20–320 μg mL−1 (R2 = 0.99998). Recovery, tested in the range of 40–120 μg mL−1, was found to be 96.1–102.1 %. Intra-day and intermediate precision RSDs ranged from 1.0–1.4 and 1.2–1.4 %, resp. The limit of detection and limit of quantitation were 0.06 and 0.20 μg mL−1, resp. The proposed technique is fast, cost-effective, reliable and reproducible, and is proposed for the routine analysis of strontium ranelate.

scholarly journals Development and Validation of Stability Indicating RP-HPLC Method for the Determination of Metaxalone in Bulk and its Pharmaceutical Formulations

2011 ◽  
Vol 8 (s1) ◽  
pp. S439-S447 ◽  
Author(s):  
Prafulla Kumar Sahu ◽  
M. Mathrusri Annapurna ◽  
Sahoo Dillip Kumar
Keyword(s):  
Dynamic Range ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Standard Curve ◽  
Oxidation Reduction ◽  
Development And Validation

A stability indicating reverse phase HPLC method was developed for the determination of metaxalone, a skeletal muscle relaxant, present in bulk and its pharmaceutical formulations using gliclazide as the internal standard (I.S). A hypersil ODS C18 column (250 × 4.6 mm, packed with 5 micron) in an isocratic mode with mobile phase Acetonitrile: phosphate buffer 3.6 (50:50%v/v) was used at a flow rate of 0.8 mL/ min and effluent was monitored at 225 nm. The assay exhibited a linear dynamic range of 0.6-100 µg/mL. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. The retention times were 5.13 min and 9.08 min for metaxalone and IS respectively. The extraction recovery of metaxalone from pharmaceutical dosage form (tablets) was >97% and the calibration curve was linear (r2= 0.999) over the entire linear range. The method had an accuracy of >98% and LOD and LOQ of 0.2 µg/mL and 0.6 µg/mL respectively. The specificity of the proposed method was performed whereby metaxalone undergoes different stress conditions like oxidation, reduction, photolysis, acid and alkaline hydrolysis.

scholarly journals Validation of an HPLC method for the simultaneous determination of eletriptan and UK 120.413

2006 ◽  
Vol 71 (11) ◽  
pp. 1195-1205 ◽  
Author(s):  
Mira Zecevic ◽  
Biljana Jocic ◽  
Snezana Agatonovic-Kustrin ◽  
Ljiljana Zivanovic
Keyword(s):  
Mobile Phase ◽  
Analytical Procedure ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Control Analysis ◽  
Internal Standard Method ◽  
Rp Hplc ◽  
Good Repeatability

Arapid and sensitive RPHPLCmethod was developed for the routine control analysis of eletriptan hydrobromide and its organic impurity UK 120.413 in Relpax? tablets. The chromatography was performed at 20?C using a C18 XTerra ? (5 ?m, 150 x 4,6 mm) column at a flow rate 1.0 ml/min. The drug and its impurity were detected at 225 nm. The mobile phase consisted of TEA (1 %) - methanol (67.2:32.8 v/v), the pH of which was adjusted to 6.8 with 85 % orthophosphoric acid. Quantification was accomplished by the internal standard method. The developed RP HPLC method was validated by testing: accuracy, precision, repeatability, specificity, detection limit, quantification limit, linearity, robustness and sensitivity. High linearity of the analytical procedure was confirmed over the concentration range of 0.05 - 1.00 mg/ml for eletriptan hydrobromide and from 0.10 - 1.50 ?g/ml for UK 120.413, with correlation coefficients greater than r = 0.995. The low value of the RSD expressed the good repeatability and precision of the method. Experimental design and a response surface method were used to test robustness of the analytical procedure and to evaluate the effect of variation of the method parameters, namely the mobile phase composition, pH and temperature. They showed small deviations from the method setting. The good recovery and low RSD confirm the suitability of the proposed RP HPLC method for the routine determination of eletriptan hydrobromide and its impurity UK 120.413 in Relpax? tables.

scholarly journals Development and validation of a rapid selective high-throughput LC-MS/MS method for the determination of triclabendazole sulfoxide concentrations in sheep plasma and its use in bioequivalence studies

2021 ◽  
Author(s):  
Lénárd Farczádi ◽  
Álmos Dósa ◽  
Orsolya Melles ◽  
Laurian Vlase
Keyword(s):  
Formic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Liver Fluke ◽  
Internal Standard ◽  
Gradient Elution ◽  
Sample Processing ◽  
Development And Validation ◽  
Analytical Separation

AbstractTriclabendazole is one of the main drugs used to treat liver fluke in livestock. A rapid LC-MS/MS method was developed and validated to determine ovine plasma levels of triclabendazole sulfoxide.A Gemini NX-C18 column was used to achieve analytical separation, with gradient elution of a mobile phase composed of 0.1% formic acid in acetonitril and 0.1% formic acid in water at flow rate of 0.6 mL/min. MRM with positive ESI ionization was used for the detection of triclabendazole sulfoxide (m/z 360.10 from m/z 376.97). Fenbendazole was used as internal standard. Plasma protein precipitation with acetonitrile was used for sample processing.The method was validated with regards to selectivity, linearity (r > 0.9939), within run and between run precision (CV < 8.9%) and accuracy (bias < 8.9%) over the concentration range 1–100 µg/mL plasma.The method developed is simple, selective and can be applied in bioequivalence and bioavailability studies.

scholarly journals Development and Validation of Estimation of Genotoxic Impurity (Hydroxylamine Hydrochloride content) in Leflunomide by using RP-HPLC technique

2021 ◽  
Vol 37 (02) ◽  
pp. 493-498
Author(s):  
Mohan Bhatale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan Ramalingam
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Hydroxylamine Hydrochloride ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
System Suitability ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, selective, linear having accuracy and specific of reverse phase high-performance liquid chromatographic (RP-HPLC) method for determination of Genotoxic impurity Hydroxylamine Hydrochloride of drug Leflunomide is reported.The separation and analysis were done on YMC Triart C18 (4.6 mm x 150 mm), having particle size 3.0 μm. KH2PO4 in 2000 mL of purified water and 2 mL triethylamine with pH 2.5 with phosphoric acid is mobile phase-A while acetonitrile is mobile Phase-B with gradient program. The elution achieved with 1.50 mL/min flow rate and using UV detection at 230 nm wavelength. Selected column oven temperature is 45°C and auto sampler 5°C respectively. In this method linearity and accuracy of Hydroxylamine HCl covered with specification limit of LOQ to 150 % (i.e.3 to 23 ppm). The observed correlation coefficient is 0.99965 and recovery in between 99.07 to 114.94. In method precision (ie.repeatability) and intermediate precision (IP) observed % RSD of six spiked test preparation is below 5.0 %. The standard and sample were stable for 3 days when stored at 2 to 8°C temperature. In robustness studies system suitability parameters ie tailing factor, theoretical plates and %RSD does not show significant changes. The present RP-HPLC method is selective, robust, linear, and precise for detection of Hydroxylamine HCl.

scholarly journals Development and Validation of RP-HPLC for Estimation of Neratinib in Bulk and Tablet Dosage Form

2019 ◽  
Vol 11 (02) ◽  
Author(s):  
M Lakshmi Kanth ◽  
B Raj Kama
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Chromatographic Separation ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Rp Hplc ◽  
Monopotassium Phosphate ◽  
Development And Validation ◽  
Tablet Dosage

An accurate RP-HPLC method developed for the estimation of Neratinib in bulk and tablet dosage form. The method is and validated for parameters linearity, accuracy, suitability, specificity, precession, LOD, LOQ and robustness. An Altima column (150 mm × 4.6 mm × 5μ) used for chromatographic separation within a runtime of 6 min. The mobile phase buffer (monopotassium phosphate) and acetonitrile (60:40 v/v) with 0.1% formic acid is used. The flow rate maintained at 1.0 ml/min with the effluents monitored at 215 nm. The Neratinib analyzed at retention time of 4.001. The concentration linear over 30-180μg/ml with regression equation y = 6065.6x + 795.43 and regression co-efficient 0.999.

Development and Validation of RP-HPLC Method for Analysis of Aclidinium Bromide and Formoterol Fumarate in Pharmaceuticals

2021 ◽  
pp. 63-69
Author(s):  
Devadasu Ch ◽  
Bharani V
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Rp Hplc ◽  
Hplc System ◽  
Standard Procedures ◽  
Aclidinium Bromide ◽  
Development And Validation ◽  
Formoterol Fumarate

A fast, sensitive, and reliable RP-HPLC method involving cyberlab HPLC System with PDA detection was developed and validated for the quantification of Aclidinium bromide and Formoterol fumarate in inhalation preparations. Chromatography was performed on the Inertsil -ODS C18 (250 x 4.6mm, 5μ) column using filtered and mixed degassed methanol: buffer (75:25 v/v) as a mobile phase with a flow rate of 1.0mL/min and the column effluent was monitored at 240nm. Retention times for Aclidinium bromide 4.713min and Formoterol fumarate 6.691min. The method obeyed linearity in the concentration range of 20-80µg/mL for the two drugs when validated according to standard procedures.

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