scholarly journals Development and validation of a reversed-phase HPLC method for determination of assay content of Teriflunomide by the aid of BOMD simulations

2021 ◽  
pp. 281-294 ◽  
Author(s):  
Abolghasem Beheshti ◽  
Zahra Kamalzadeha ◽  
Monireh Haj-Maleka ◽  
Meghdad Payaba ◽  
Mohammad Amin Rezvanfar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Td Dft ◽  
High Level ◽  
Development And Validation

Due to the new hopes for treatment of multiple sclerosis (MS) diseases by Teriflunomide (TFN), in this project, a cheap, robust, and fully validated method has been developed both for determination of assay content in API (active pharmaceutical ingredient), and for related impurities analysis (RIA). To operate the method, a common C18, end-capped (250 × 4.6) mm, 5µm liquid chromatography column, was applied. The mobile phase A was prepared by dissolving 2.74 g (20mM) of PDP (potassium dihydrogen phosphate) and 3.72 g (50mM) of PC (potassium chloride) in water (1000 mL). Then, pH was adjusted to 3.0 by adding OPA (ortho-phosphoric acid) 85%; while, the mobile phase B was acetonitrile (ACN) (100%). In order to confirm the experimental data about the λmax of TFN, we have used the Born-Oppenheimer molecular dynamics (BOMD) simulations, quantum mechanics (QM), and TD-DFT calculations. According to the results, the method showed a high level of suitability, specificity, linearity, accuracy, precision, repeatability, robustness, and reliable detection limit.

scholarly journals Development and validation of a fast, simple, cost-effective and robust HPLC method for lisinopril determination in solid pharmaceutical dosage forms

2017 ◽  
Vol 36 (2) ◽  
pp. 201 ◽  
Author(s):  
Tanja Bakovska Stoimenova ◽  
Marjan Piponski ◽  
Gordana Trendovska Serafimovska ◽  
Marina Stefova
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Cost Effective ◽  
Dosage Forms ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Forms ◽  
Operational Conditions ◽  
Development And Validation

A fast, simple, cost-effective and robust chromatographic method was developed and validated for determination of the antihypertensive drug lisinopril dihydrate in tablets under routine operational conditions, without ion-pair reagents, high column temperatures and an acidic mobile phase. Taking into consideration all four different pKa values of lisinopril, the separation was optimized using the C18 column (end-capped, 150 mm × 4.6 mm 5 µm) and a mobile phase composed of methanol and ammonium (or potassium) dihydrogen phosphate buffer (pH 7.2) with a flow rate of 1.1 ml/min, UV detection at 214 nm and a temperature of 40 °C. These optimized conditions led to the production of a single and symmetrical peak for lisinopril. This mobile phase is suitable for different HPLC columns, which makes it appropriate for industrial quality control laboratories. The developed method was validated, showing excellent validation results and the possibility to be implemented for the determination of lisinopril in combined dosage forms with other active substances.

scholarly journals Simultaneous HPLC Determination of Chlordiazepoxide and Mebeverine HCl in the Presence of Their Degradation Products and Impurities

2015 ◽  
Vol 2015 ◽  
pp. 1-9
Author(s):  
Rania N. El-Shaheny ◽  
Fathalla F. Belal
Keyword(s):  
Simultaneous Determination ◽  
Degradation Product ◽  
Mobile Phase ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Ir Studies ◽  
Validation Procedure

A simple, rapid, and sensitive RP-HPLC method was developed and validated for the simultaneous determination of chlordiazepoxide (CDO) and mebeverine HCl (MBV) in the presence of CDO impurity (2-amino-5-chlorobenzophenone, ACB) and MBV degradation product (veratric acid, VER). Separation was achieved within 9 min on a BDS Hypersil phenyl column (4.5 mm × 250 mm, 5 µm particle size) using a mobile phase consisting of acetonitrile: 0.1 M potassium dihydrogen phosphate: triethylamine (35 : 65 : 0.2, v/v/v) in an isocratic mode at a flow rate of 1 mL/min. The pH of the mobile phase was adjusted to 4.5 with orthophosphoric acid and UV detection was set at 260 nm. A complete validation procedure was conducted. The proposed method exhibited excellent linearity over the concentration ranges of 1.0–100.0, 10.0–200.0, 2.0–40.0, and 2.0–40.0 µg/mL for CDO, MBV, VER, and ACB, respectively. The proposed method was applied for the simultaneous determination of CDO and MBV in their coformulated tablets with mean percentage recoveries of 99.75 ± 0.62 and 98.61 ± 0.38, respectively. The results of the proposed method were favorably compared with those of a comparison HPLC method using Studentt-test and the variance ratioF-test. The chemical structure of MBV degradation product was ascertained by mass spectrometry and IR studies.

scholarly journals Validation of Simultaneous Volumetric and HPLC Methods for the Determination of Pridinol Mesylate in Raw Material

2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Laura D. Simionato ◽  
Leonardo Ferello ◽  
Sebastián Stamer ◽  
Patricia D. Zubata ◽  
Adriana I. Segall
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Volumetric Method ◽  
Raw Material ◽  
Organic Layer ◽  
Dihydrogen Phosphate ◽  
Reverse Phase ◽  
Potassium Dihydrogen

Simple, sensitive, and economical simultaneous volumetric and HPLC methods for the determination of pridinol mesylate in raw material have been developed. The volumetric method is based on the reaction of pridinol with sodium lauryl sulphate in diluted sulphuric acid. Dimethyl yellow was used as indicator to detect the end point of the titration in aqueous/organic layer. The HPLC method for the determination of pridinol mesylate employs a reverse phase C18 column at ambient temperature with a mobile phase consisting of acetonitrile: 0.05 M potassium dihydrogen phosphate, pH adjusted to 5.0 (1 : 2, v/v). The flow rate was 0.8 mL/min. Quantitation was achieved with UV detection at 258 nm based on peak area. Both methods were found to be suitable for the quality control of pridinol mesylate in raw material.

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 a Reversed-Phase HPLC Method for Determination of Alkaloids from Papaver somniferum L. (Papaveraceae)

2012 ◽  
Vol 95 (2) ◽  
pp. 399-405 ◽  
Author(s):  
Jelena Acevska ◽  
Aneta Dimitrovska ◽  
Gjoshe Stefkov ◽  
Katerina Brezovska ◽  
Marija Karapandzova ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Ph Value ◽  
Reversed Phase ◽  
Hplc Method ◽  
Papaver Somniferum ◽  
Chromatographic Behavior ◽  
Organic Modifier ◽  
Column Temperature ◽  
Development And Validation

Abstract An HPLC method for the separation of six target alkaloids from Papaver somniferum L. (morphine, codeine, oripavine, thebaine, papaverine, and noscapine) was developed, optimized, and validated. The chromatographic behavior of these alkaloids was investigated using a reversed-phase chromatography at acidic and alkaline pH. The effects of ion-pairing agents, pH value of the mobile phase, concentration of the buffer components, mobile phase organic modifier, and column temperature were studied. Regardless of the large differences in their pKa values, all alkaloids were separated within a close retention window, and good peak shape was achieved for each of the six alkaloids. The proposed method has adequate selectivity, linearity, accuracy, precision, and reproducibility and is applicable for poppy straw.

scholarly journals Development and Validation of RP-HPLC Method for Estimation of Teneligliptin and its Impurity in Tablet

2021 ◽  
Vol 69 (02) ◽  
Author(s):  
Bhoomi Dineshkumar Patel ◽  
Nidhi J. Dharsandiya ◽  
Ankit Chaudhary
Keyword(s):  
Present Method ◽  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Development And Validation ◽  
Tablet Dosage

The objective of the study is a simple, precise and accurate stability RP-HPLC method has been developed and subsequently validated for the estimation of Teneligliptin and its impurity in tablet formulation. The adequate separation was carried out using Grace Smart C18 column (250mm x 4.6mm, 5?m particle size), mixture of 0.05M Potassium dihydrogen phosphate PH 4.0 and Acetonitrile 80:20 % v/v as a mobile phase with a flow rate of 1 ml/min and the effluent was monitored at 242 nm using PDA detector. The retention time of Teneligliptin, Impurity B and Impurity G were 7.443 min, 6.650 min and 8.473 min respectively. Linearity for Teneligliptin, Impurity B and Impurity G were found in the range of 500-3000 µg/ml (R2 = 0.998), 5-15 µg/ml (R2 = 0.994) and 5-15 µg/ml (R2 = 0.998) respectively. The accuracy of the present method was evaluated at 50%, 100% and 150%. The % recoveries of drug were found to be in range of 99.315 ± 0.283 for Teneligliptin. Precision studies were carried out and the RSD values were less than two. The method was found to be robust. The proposed method was found to be specific, accurate, precise and robust can be used for simultaneous estimation of these drugs in tablet dosage form.

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.

scholarly journals Robust and Fast UV–HPLC Method for Biotransformation Analysis of Azecines

2021 ◽  
Vol 84 (3) ◽  
pp. 275-283
Author(s):  
Stephanie Zergiebel ◽  
Andreas Seeling
Keyword(s):  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Chromatographic Separations ◽  
Drug Candidates ◽  
Lack Of Information ◽  
Gastrointestinal Fluid

AbstractDibenzoazecines are a new class of drug candidates for the treatment of schizophrenia. Compared to the drugs currently used in therapy, the azecines have a novel mechanism of action. Thus, they have the potential to cause fewer side effects compared to the standard therapy with a constant high neuroleptic potency. This theory was substantiated by comparative in vivo tests with haloperidol and risperidone. Seventeen new azecine derivatives have already been tested furthermore of stability, physicochemical parameters, pharmacokinetics including esterase cleavage, stability in simulated gastrointestinal fluid, stability at different pH values and determination of octanol/water-partition coefficients. For these substances, class is still a lack of information concerning the metabolism. Therefore, the present study investigated and developed a reliable and reproducible gradient reversed-phase HPLC–UV method to determinate the lead structure LE404 alongside emerging metabolites in compliance with international requirements like ICH guidelines and the European Pharmacopoeia. Up to now, there is no innovative method suitable for such a determination. Chromatographic separations were achieved with a phenomenex™ Gemini column (5 µm C18 110 Å, 250 × 4.60 mm) using a mixture of acetonitrile/potassium dihydrogen phosphate buffer (4 mmol L−1, pH 2.5) as mobile phase. The gradient method flow rate was 1.0 mL min−1, and UV detection was made at 220 nm. The optimized HPLC method was found to be specific, accurate, reproducible and robust for determination of LE404.

scholarly journals A Rapid Reversed-Phase HPLC Method for Analysis of Trans-Resveratrol in PLGA Nanoparticulate Formulation

2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Gurinder Singh ◽  
Roopa S. Pai
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Potassium Dihydrogen Phosphate ◽  
Plga Nanoparticles ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Relative Standard ◽  
New Formulation

A rapid reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of trans-resveratrol (t-RVT) in PLGA nanoparticle formulation. A new formulation of t-RVT loaded PLGA nanoparticles (NPs) with potential stealth properties was prepared by nanoprecipitation method in our laboratory. The desired chromatographic separation was achieved on a Phenomenex C18 column under isocratic conditions using UV detection at 306 nm. The optimized mobile phase consisted of a mixture of methanol: 10 mM potassium dihydrogen phosphate buffer (pH 6.8): acetonitrile (63 : 30 : 7, v/v/v) at a flow rate of 1 mL/min. The linear regression analysis for the calibration curves showed a good linear correlation over the concentration range of 0.025–2.0 μg/ml, with determination coefficients, R2, exceeding 0.9997. The method was shown to be specific, precise at the intraday and interday levels, as reflected by the relative standard deviation (RSD) values, lower than 5.0%, and accurate with bias not exceeding 15% and percentage recovery was found to be in the range between 94.5 and 101.2. The limits of detection and quantification were 0.002 and 0.007 μg/ml, respectively. The method was successfully applied for the determination of t-RVT encapsulation efficiency.

scholarly journals Development and Validation of RP-HPLC Method for Quantitation of Clarithromycin in Matrix Tablet Dosage Form

2017 ◽  
Vol 16 (1) ◽  
pp. 69-75 ◽  
Author(s):  
Md Mahbubul Alam ◽  
Md Shahadat Hossain ◽  
Subrata Bhadra ◽  
Uttom Kumar ◽  
Abu Shara Shamsur Rouf
Keyword(s):  
Dosage Form ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Matrix Tablet ◽  
Uv Detector ◽  
Rp Hplc ◽  
Development And Validation ◽  
Tablet Dosage

This study was aimed to develop a simple, sensitive and rapid procedure for the analysis of clarithromycin in pure as well as in matrix tablet dosage form by using RP-HPLC method. The chromatographic separation was achieved by a reversed phase C18 column (150 mm length × 4.6 mm i.d., 5 ?m particle size) in an isocratic mode with mobile phase comprising of acetonitrile and 0.035 M potassium dihydrogen phosphate (pH 4.4 ± 0.017) in a ratio of (55: 45, v/v). The eluent was pumped at a flow rate of 0.6 ml/min and the effluent was monitored using UV detector at 210 nm. The method was validated according to the ICH guidelines with respect to linearity, precision, accuracy, selectivity, specificity, ruggedness and robustness. It was found to be linear over the concentration range of 320- 480 ?g/ml (R2= 0.9993) with detection limit of 0.04 ?g/mL. Considering the specifications of this method, the system was found to be suitable for rapid and routine analysis of clarithromycin in pure and matrix tablet dosage form.Dhaka Univ. J. Pharm. Sci. 16(1): 69-75, 2017 (June)

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