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 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 Estimation of Genotoxic Impurity (Benzimidamidecontent) in Leflunomide by Using RP-HPLC Technique

2021 ◽  
pp. 78-85
Author(s):  
Mohan Bhatale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan Ramalingam
Keyword(s):  
High Performance ◽  
Room Temperature ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Program Mode

The measurement of Genotoxic contaminant, a simple, selective, linear, accurate, and specific reverse phase high-performance liquid chromatographic (RP-HPLC) process was proposed. A Benzimidamide impurity in the medication Leflunomide has been discovered. Separation and analysis were carried out on Zorbax SB phenyl (4.6 mm x 250 mm) with a particle size of 5.0 μm. with 0.1 % Triethylamine in purified water with a pH of 7.0 and a buffer of phosphoric acid (20% in water). The mobile phase is a 40:60 mixture of buffer and Acetonitrile with degassing. Isocratic program mode was used. The elution was carried out at a rate of 1.0 mL/min with UV detection at a wavelength of 289 nm. The temperature of the selected column oven is 25°C. The linearity and accuracy of Benzimidamide are covered in this approach, with a LOQ limit of 150 percent (i.e.0.03 to 0.45 ppm). The observed correlation coefficient is 0.99994, with a range of 100.01 to 104.8 for recovery. The measured percent RSD of six spiked test preparation is below 5.0 percent in procedure precision (i.e. repeatability) and intermediate precision (IP). When maintained at room temperature, the standard and sample remained stable for three days. System appropriateness characteristics such as tailing factor and percent RSD do not exhibit significant changes in robustness experiments. For the detection of Benzimidamide the present RP-HPLC method is act as selective, robust, linear and precise.

scholarly journals Development and validation for determination of lisinopril dihydrate in bulk drug and formulation using RP-HPLC method

2018 ◽  
Vol 3 (2) ◽  
pp. 14-18
Author(s):  
Zahid Zaheer ◽  
Sarfaraz Khan ◽  
Mohammad Sadeque ◽  
Hundekari G. I. ◽  
Rana Zainuddin
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Rp Hplc ◽  
Liquid Chromatographic Method ◽  
Bulk Drug ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Isocratic Mode

A simple, reproducible and efficient reverse phase high performance liquid chromatographic method was developed for Lisinopril in bulk drug and formulation. A column having 150 × 4.6 mm in isocratic mode with mobile phase containing acetonitrile: phosphate buffer (70:30; adjusted to pH 3.0) was used. The flow rate was 0.8 ml/min and effluent was monitored at 216 nm. The retention time (min) and linearity range (μg/ml) for Lisinopril was (1.510) and (10-35). The developed method was found to be accurate, precise and selective for determination of Lisinopril in bulk and formulation.

scholarly journals DEVELOPMENT AND VALIDATION OF A HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD DETERMINATION OF ZIDOVUDINE ENCAPSULATED IN PCL NANOPARTICLES

2017 ◽  
Vol 1 (2) ◽  
pp. 1-8
Author(s):  
Milena Cristina Ribeiro Souza Magalhães ◽  
Alisson Samuel Portes Caldeira ◽  
Hanna De Sousa Rocha Almeida ◽  
Sílvia Ligório Fialho ◽  
Armando Da Silva Cunha Junior
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Isocratic Mode

A reversed-phase high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of encapsulation efficiency of zidovudine in nanoparticules. The method was carried out in isocratic mode using 0.040M sodium acetate: methanol: acetonitrile: glacial acetic acid (880:100:20:2) as mobile phase, a C8 column at 25ºC and UV detection at 240 nm. The method was linear (r2 ˃ 0.99) over the range of 25.0-150.0 μg/mL, precise (RSD ˂ 5%), accurate (recovery = 100.5%), robust and selective. The validated HPLC-UV method can be successfully applied to determine the rate of zidovudine in nanoparticules.

Development and Validation of RP-HPLC Method for Simultaneous Estimation of Gatifloxacin and flurbiprofen Sodium in Eye Drops

2019 ◽  
Vol 9 (01) ◽  
pp. 83-88
Author(s):  
Pinkal Patel ◽  
Nalini Patel ◽  
Kinjal Parmar
Keyword(s):  
High Performance ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Eye Drops ◽  
Rp Hplc ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple, selective and rapid reversed phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed and validated for the simultaneous analysis Gatifloxacin and flurbiprofen sodium in eye drops. The separation was carried out using a mobile phase consisting ACN: Buffer (pH 3.5) in the ratio of 55:45 v/v. The column used was Phenomenex luna ODS C18 (250mm X 4.6 mm i.d., 5 μm particle size) with flow rate of 1 ml / min using UV detection at 268 nm. The described method was linear over a concentration range of 2-12 μg/ml for both of Gatifloxacin and flurbiprofen sodium. The retention times of Gatifloxacin and flurbiprofen sodium were found to be 3.710 min. and 6.797 min respectively. Method was validated statistically and recovery studies were carried out. The proposed method has been applied successfully to the analysis of cited drugs either in pure form or in pharmaceutical formulations with good accuracy and precision. The method here in described can be employed for quality control and routine analysis of drugs in pharmaceutical formulations.

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OFTRANDOLAPRIL AND VERAPAMIL IN COMBINED TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (05) ◽  
pp. 61-64
Author(s):  
A. L Rao ◽  
◽  
R. V Bhaskara
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Liquid Chromatographic

A reverse phase high performance liquid chromatographic method was developed and validated asper ICH guidelines for estimation of trandolapril and verapamil in combined tablet dosage form. Theseparation was obtained using a mobile phase consisting of acetonitrile and phosphate buffer adjustingpH to 3.0 in the ratio of 70:30 v/v and using Waters C18 (250 x 4.6 mm, 5 mcm) column maintained atambient temperature. The flow rate was 1.2 mL min-1 and UV detection was monitored at 215 nm. Theretention time (min) and linearity range (mcg mL-1) for trandolapril and verapamil were (5.12, 2.70) and(20-60, 20-60), respectively. The method validation results are within the acceptance criteria for precision,accuracy and linearity. The proposed method was found to be suitable for routine quality control ofmarketed formulation containing these APIs.

Stereospecific Determination of Sertraline and its Impurities in Bulk Drug Using Cyclodextrins as a Chiral Selector

2020 ◽  
Vol 16 (7) ◽  
pp. 823-830 ◽  
Author(s):  
Navjot Kaur Sandhu ◽  
Durga Das Angehore ◽  
Neeraj Upmanyu ◽  
Pawan K. Porwal
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Related Substances ◽  
System Suitability ◽  
Bulk Drug ◽  
Liquid Chromatographic

Background: Sertraline Hydrochloride, an oral anti-depressant, has two chiral centers and its cis enantiomers and trans diasteromers are defined as related substances by United State Pharmacopoeia and British Pharmacopoeia. Introduction: A selective, stereospecific and economical high performance liquid chromatographic (HPLC) method was developed for the determination of sertraline enantiomeric forms. The HPLC-UV method was developed and optimized in the terms of system suitability parameters. Methods: The elution was made using a mixture of -cyclodextrin (-CD) and hydroxypropyl - cyclodextrin (HP -CD). Analysis was performed on a Zorbax SB C-18 column (250 x 4.6mm), 5μ with the mobile phase consisting of 170mM KH2PO4 containing -CD and HP -CD (pH: 3.0 with dil. H3PO4) and acetonitrile (75:25, v/v). Flow rate was kept at 1.0mL/min and the detection was carried out by UV at 220nm. Enantio-separation for sertraline was carried out using two different CDs (β-CD and HP β- CD) at different concentrations in the mobile phase. Results: Complete resolution of all the four isomers was achieved using 9mM β-CD and 15mM HP β- CD in the mobile phase. The development was optimized using central composite quadric model, where concentration of -CD and HP -CD were varied and resolution between trans diastereomeric impurities was calculated as a response. Conclusion: Resolution between any pair of isomers was found to be more than 2. Method development and optimization leading to the best resolution between the isomers of sertraline is described in detail.

scholarly journals Analytical Method Development and Validation for the Estimation of Canagliflozin in Bulk and Formulation by RP- HPLC

2018 ◽  
Vol 10 (03) ◽  
Author(s):  
Darshan Bhatt ◽  
Padmini Thatavarthi ◽  
B. Rajkamal
Keyword(s):  
High Performance ◽  
Chromatographic Method ◽  
Method Development ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Rp Hplc ◽  
Limit Of Quantitation ◽  
Development And Validation ◽  
Liquid Chromatographic

A simple and sensitive reverse phase high performance liquid chromatographic method was developed and successively validated for the estimation of Canagliflozin. In the new method, Canagliflozin separation was carried out by the nonpolar inertsil ODS-3 (250 × 4.6 mm, 5μ) column with a mobile phase composition of Ammonium acetate buffer (pH-4.5) and Acetonitrile in the ratio of 30:70% v/v. Canagliflozin was determined at 252 nm using UV detection and the compound was eluted at the retention time of 4.5 min. As per International Conference on Harmonization (ICH) guidelines, the method was validated and the parameters were precision, accuracy, linearity, limit of detection, limit of quantitation and robustness. The chromatographic method was accurate, linear, specific, precise and robust. The results of method concluded that the proposed RP-HPLC method is useful, convenient and reliable in regular analysis of Canagliflozin in bulk and its formulation

scholarly journals Isocratic RP-HPLC Method for Simultaneous Separation and Estimation of Zofenopril and Hydrochlorthiazide in Pharmaceutical Dosage Forms

2012 ◽  
Vol 9 (2) ◽  
pp. 999-1006 ◽  
Author(s):  
G. S. Devika ◽  
M. Sudhakar ◽  
J. Venkateshwara Rao
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Sodium Hydroxide Solution ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Simultaneous Separation ◽  
Liquid Chromatographic

A simple, rapid, sensitive and accurate isocratic reverse phase high performance liquid chromatographic (RP-HPLC) method has been developed and subsequently validated for the simultaneous determination of Zofenopril and Hydrochlorthiazide in combined dosage form. Chromatographic separation of the two drugs was performed on a Purospher BDS C18 column (250 mm × 4.6 mm id, 5 μm particle size). The mobile phase comprising of acetonitrile methanol: 0.02M NaH22PO4buffer (40:20:40) was delivered at a flow rate of 1.0mL/min. The pH of the mobile phase is adjusted to 7.2 with Sodium hydroxide solution. Detection was performed at 245 nm.The separation was completed within 10 min and the retention time of hydrochlorthiazide is 4.62 and Zofenopril is 6.86 min respectively. Calibration curves were linear with R2between 0.99-1.0 over a concentration range of 100-600 μg/ml for Zofenopril calcium and 50-300 μg/ml for hydrochlorthiazide..The developed method was successfully applied to determi

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