scholarly journals Development and Validation of RP-HPLC Method for Desoximetasone in Bulk and Cream Formulation

2019 ◽  
Vol 9 (3) ◽  
pp. 154-159
Author(s):  
Ashish Gorle ◽  
Jayashri Mahajan ◽  
Prathamesh Bhave
Keyword(s):  
Method Validation ◽  
Mobile Phase ◽  
High Performance ◽  
Gradient Elution ◽  
Hplc Method ◽  
Topical Steroids ◽  
Cream Formulation ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Development And Validation

Desoximetasone chemically is 9-fluoro-IIβ21-dihydroxy-I6a-methylpregna-I.4-diene-3.The precise mechanism of the anti-inflammatory activity of topical steroids in the treatment of steroid-responsive dermatoses, in general, is uncertain. So, in present investigation chromatographic methods were developing use RP-HPLC for estimation of Desoximetasone in bulk and in cream formulation and method validation according to ICH guidelines. The main objective of this study was to develop a simple and reproducible method for desoximetasone by Reverse Phase High Performance Liquid Chromatography (RP-HPLC). In this work the desoximetasone separation was carried out by using C18 cosmosile column (250mmx4.6mm particle size 5µm). By using 0.1% orthrophosphoric acid pH adjusted up to 3 at uv detection of 240nm.The mobile phase was used at various ratio for gradient elution the ratio of mobile phase was 20:80 v/v. Methanol and water used for mobile phase and flow rate was being set at 1mL/min. The linearity of proposed method was found in range of r =0.9989. Statistically validation parameters such as linearity, accuracy, precision, LOD and LOQ were checked. Keywords: Desoximetasone, RP-HPLC, Method validation.

scholarly journals Analytical Method Development and Validation of Rp-Hplc Method for Simultaneous Estimation of Pyridoxamine Dihydrochloride and Acetylcysteine in Tablet Dosage Form.

2021 ◽  
Vol 23 (06) ◽  
pp. 992-1000
Author(s):  
Sneha S. Ghule ◽  
◽  
Ashpak M. Tamboli ◽  
Snehal D. Patil ◽  
◽  
...  
Keyword(s):  
High Performance ◽  
Method Development ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
System Suitability ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Tablet Dosage

A reverse-phase high-performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of Pyridoxamine dihydrochloride and Acetylcysteine in the marketed formulation is developed. Chromatography carried out at 30oc temperature on Agilent Zorbax Bonus-RP (250 x 4.6 mm, 5 µ) coloum. Coloum using a mobile phase 0.1% trifluroacetic acid in water: acetonitrile (80:20v/v) with flow rate 1ml/min (DAD scan at 210nm). Validation parameters such as system suitability, linearity, precision, accuracy are considered as reported International Conference on Harmonization guidelines. The retention times for Pyridoxamine dihydrochloride and Acetylcysteine are 2 min and 3.4 min. The linearity range for Pyridoxamine dihydrochloride and Acetylcysteine is 30-70 µg/ml and 180-420 µg/ml. The %RSD for accuracy was found to be less than 2%. Hence the proposed method was found to be accurate, precise, reproducible, and specific and can be used for simultaneous analysis of these drugs in tablet formulation.

scholarly journals Qualitative and quantitative evaluation of melittin in honeybee venom and drug products containing honeybee venom

2013 ◽  
Vol 57 (2) ◽  
pp. 37-44 ◽  
Author(s):  
Ghasem Haghi ◽  
Alireza Hatami ◽  
Mehdi Mehran
Keyword(s):  
High Performance ◽  
Pure Water ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Honeybee Venom ◽  
Drug Products ◽  
Rp Hplc ◽  
Validation Parameters ◽  
Main Component

Abstract A reverse-phase high-performance liquid chromatographic (RP -HPLC ) method was developed and validated for the analysis of honeybee venom samples and drug products containing honeybee venom. The validation parameters were linearity, sensitivity, precision, and recovery. Melittin is the main component of honeybee venom was extracted with pure water, and then evaluated by RP -HPLC with a photodiode array (PDA ) detector. Separation of the samples was achieved on a Europa Protein C18 column with linear gradient elution of acetonitrile and 0.4% phosphoric acid at 25°C. There was a flow rate of 1 mL/min. Detection was set at 220 nm. Limits of detection (LOD ) and quantification (LO Q) for melittin were 1.1 and 3.2 μg/mL, respectively. The amount of melittin in honeybee venom samples ranged from 21.9 to 66.4 %.

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 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 A New Quantitative Analytical Method Development and Validation for the Analysis of Boceprevir in Bulk and Marketed Formulation

2018 ◽  
Vol 10 (03) ◽  
Author(s):  
Bhetanabotla Chandramowli ◽  
B.M Syam Kumar ◽  
D.V. R. N. Bhikshapathi ◽  
Bigala B Rajkamal
Keyword(s):  
Chromatographic Analysis ◽  
Mobile Phase ◽  
Method Development ◽  
Hplc Method ◽  
Capsule Formulation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Method Development And Validation ◽  
Development And Validation

A simple, precise and accurate RP-HPLC technique was developed and the developed method was validated for the regular analysis of Boceprevir. Chromatographic analysis was performed by selecting X-Terra ODS ( C18) column (4.6 mm i.d. × 250 mm, 5μ), Acetonitrile : Phosphate buffer pH -3 ( 90 : 10% v/v) as mobile phase, 1.0 ml/min as flow rate and 20μl injection volume. The LC chromatographic peak was eluted at 3.6 min at 235 nm as UV detection wavelength. The developed method was validated as per the ICH guidelines and the Validation parameters were specificity, accuracy, linearity, precision, LOD and LOQ. Linear relationship for Boceprevir established in the concentration range of 50 to 150μg/mL. Accuracy in terms of percentage recovery found in the range between 98 to 101%. LOD and LOQ values were found to be 2.3 and 7.123μg/mL respectively. The results of the method established that the new RP-HPLC method is convenient and simple in regular analysis of Boceprevir in bulk and capsule formulation.

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

2021 ◽  
Vol 37 (2) ◽  
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 method for the estimation of omeprazole in bulk and capsule dosage forms

2012 ◽  
Vol 1 (11) ◽  
pp. 366-369 ◽  
Author(s):  
Kalakonda Sri Nataraj ◽  
Mohammad Badrud Duza ◽  
Kalyani Pragallapati ◽  
Dussa Kiran Kumar
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Accurate Method ◽  
Pharmaceutical Journal ◽  
Dosage Forms ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Development And Validation

A method for the determination of omeprazole in bulk and capsule dosage form by reverse phase high performance liquid chromatography has been developed. This is a simple, rapid, precise and an accurate method. The method was developed on a Novapak C18, (250 x 4.6 mm, 5µ) column using phosphate buffer (pH 7.4) and acetonitrile in the ratio of 60:40, v/v as a mobile phase which was pumped at a flow rate of 1.0 ml/min and detection was done at 302 nm. The retention time of the drug was found to be 7.71 min. The method was validated for accuracy, precision, linearity, specificity, robustness. The linearity was observed in the range of 20-60 ppm. The results of recovery studies indicated that the method was accurate. Hence the developed method was found to be suitable for the estimation of omeprazole in bulk and capsule dosage forms.DOI: http://dx.doi.org/10.3329/icpj.v1i11.12062 International Current Pharmaceutical Journal 2012, 1(11): 366-369

scholarly journals A NOVEL ANALYTICAL METHOD FOR SIMULTANEOUS QUANTIFICATION OF DAPAGLIFLOZIN AND SITAGLIPTIN BY REVERSE PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2021 ◽  
Vol 10 (3) ◽  
pp. 2861-2865
Author(s):  
Ajay Gupta
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
High Performance ◽  
Potassium Phosphate ◽  
Cost Effective ◽  
Gradient Elution ◽  
Hplc Method ◽  
Reverse Phase ◽  
Simultaneous Quantification ◽  
Validation Parameters

The Reverse phase HPLC method was developed for simultaneous determination of Dapagliflozin and Sitagliptin in single analytical method. Chromatographic separation was achieved on a Hypersil BDS C18 (250mmx4.6mm, 5µm) column applying an gradient elution based on potassium phosphate monobasic buffer pH (3.0) as mobile phase A while methanol and acetonitrile in the ratio of (60:40 v/v) as a mobile phase B with gradient program Time/Mobile phase A%/Mobile phase B% is as 0 min./55/45, 3 min./55/45, 9 min./20/80, 13 min.20/80, 15 min./55/45, 20 min./55/45. Validation parameters specificity, linearity, accuracy, precision and robustness have been observed to be desirable over the concentration ranges of 50-150 µg/ml for Dapagliflozin and Sitagliptin respectively. All the variables have been studied to optimize the chromatographic conditions. The optimized approach verified through validation and confirmed to be the intended purpose for the quality control of the mentioned drugs, as per ICH guidelines. For simultaneous quantification of Dapagliflozin and Sitagliptin, the developed method was found to be genuinely exact precise, accurate, linear, fast, and cost effective.

scholarly journals Method Development and Validation of Polmacoxib in Capsule Dosage Form by RP-HPLC

2021 ◽  
Vol 11 (4-S) ◽  
pp. 59-63
Author(s):  
Anjali Chaudhary ◽  
Meenakshi Dhaiya ◽  
Shaily Tyagi ◽  
Swati Mittal
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Hplc Method ◽  
Rp Hplc ◽  
Method Development And Validation ◽  
Development And Validation ◽  
Intended Use

A simple and sensitive RP-HPLC method developed for estimation of Polmacoxib in bulk by using a high performance liquid chromatography with PDA detector using Phenomenex luna C18 column (250mmx4.6mm), 5 µm; mobile phase comprises of Water : ACN as (1:1) at the flow rate 1.0 ml/min and the wavelength of detection  238 nm and eluted at 8.12 minutes. The proposed method is validated for specificity, Linearity, Precision, accuracy, ruggedness, and Robustness. All the parameters were found within the acceptable limits. RP-HPLC method was a simple, reliable economic and acceptable and it confirmed that method is suitable for the intended use for routine quality control and assay of drugs. This method is successfully applied for the determination of commercial dosage form capsule preparation. This method is validated as per ICH (International conference on harmonization) Guidelines. Keywords: Polmacoxib, RP-HPLC, ICH, PDA Detector, Precision

scholarly journals SIMULTANEOUS DETERMINATION OF DIPHENHYDRAMINE, EPHEDRINE, NOSCAPINE, AND GLYCEROL GLYCOLATE USING STABILITY-INDICATING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY: APPLICATION TO NOSCOF TABLETS

2019 ◽  
pp. 505-511
Author(s):  
PULAGURTHA BHASKARARAO ◽  
GOWRI SANKAR DANNANA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Uv Light ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Validation Parameters

Objective: Noscof tablet is a fixed dosage combination formulation having diphenhydramine (DH), ephedrine (ED), noscapine (NP), and glycerol glycolate (GG). A sensitive, selective, accurate, precise, and stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) method with photodiode array detection has been developed and validated for simultaneous analysis of DH, ED, NP, and GG in bulk drug and Noscof tablets. Methods: Reversed-phase chromatographic separation and analysis of DH, ED, NP, and GG were done on an Altima C18 column with 0.01 M KH2PO4 buffer (pH 3.5) and acetonitrile (50:50%, v/v) as mobile phase at 0.8 ml/min flow rate in isocratic mode. Detection was performed at 260 nm. The method was validated in harmony with International Conference on Harmonization (ICH) guidelines. The tablet sample solution was subjected to diverse stress conditions using ICH strategy such as hydrolytic degradation (neutral - with distilled water, alkaline - with 2 N NaOH, and acidic - with 2 N HCl), oxidation (with 10% H2O2), photodegradation (exposing to UV light), and dry heat degradation (exposing to 105°C). Results: Using the above stated chromatographic conditions, sharp peaks were obtained for ED, NP, DH, and GG with retention time of 3.272 min, 4.098 min, 5.467 min, and 6.783 min, respectively. Good regression coefficient values were obtained in the range of 2–12 μg/ml for ED, 3.75–22.5 μg/ml for NP, 3.125–18.75 μg/ml for DH, and 25–150 μg/ml for GG. The quantification limits were 0.181 μg/ml, 0.187 μg/ml, 0.246 μg/ml, and 1.114 μg/ml for ED, NP, DH, and GG, respectively. The values of validation parameters are within the acceptance limits given by ICH. The ED, NP, DH, and GG showed more percent of degradation in acid condition and less percent of degradation in the neutral condition. The peaks of degradants did not interfere with the peaks of analytes. ED, NP, DH, and GG were assessed with a good percentage of the assay (near to 100%) and low percent relative standard deviation (<2%) in Noscof tablets using the proposed method. Conclusion: The stability indicating RP-HPLC method developed was suitable for quantifying ED, NP, DH, and GG simultaneously in bulk as well as in tablet formulation.

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