Development of an Ion-Pair Reversed-Phase HPLC Method with Indirect UV Detection for Determination of Phosphates and Phosphites as Impurities in Sodium Risedronate

Abstract A method based on RP-HPLC with indirect UV detection was developed for the determination of phosphates and phosphites as impurities in sodium risedronate. RP separation of the phosphates and phosphites was achieved by adding tetrabutylammonium hydroxide as an ion-pairing agent in the mobile phase. Potassium hydrogen phthalate was added to the mobile phase as an ionic chromophore in order to obtain high background absorption of the mobile phase. Separation was performed on a C18 column using a mixture of pH 8.2 buffer (containing 0.5 mM tetrabutylammonium hydroxide and 1 mM phthalate) and acetonitrile (95 + 5, v/v) as the mobile phase, with indirect UV detection at 248 nm. The validation of the method included determination of specificity/selectivity, linearity, LOD, LOQ, accuracy, precision, and robustness. The LOD was 0.86 g/mL for phosphates and 0.76 g/mL for phosphites. The LOQ was 2.60 g/mL for phosphates and 2.29 g/mL for phosphites. The developed method is suitable for quantitative determination of phosphates and phosphites as impurities in QC of sodium risedronate.

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RP-HPLC method with indirect UV detection for determination of sodium ibandronate in pharmaceuticals

Macedonian Pharmaceutical Bulletin ◽

10.33320/maced.pharm.bull.2018.64.02.005 ◽

2019 ◽

Vol 64 (02) ◽

pp. 43-49

Author(s):

Zharko Tanturovski ◽

Zorica Arsova-Sarafinovska ◽

Aneta Dimitrovska

Keyword(s):

Sodium Salt ◽

Pharmaceutical Formulations ◽

Reversed Phase ◽

Hplc Method ◽

Uv Detection ◽

Array Detector ◽

Ibandronic Acid ◽

Indirect Uv Detection ◽

Rp Hplc

Ibandronate sodium (IBN) [(1-hydroxy-3- (methyl pentyl amino) propylidene bisphosphonic acid monosodium monohydrate)] is the sodium salt of ibandronic acid, a synthetic nitrogen-containing bisphosphonate drug. The aim of this study was to develop a sensitive and accurate RP-HPLC method with indirect UV detection for determination of IBN in pharmaceutical formulations. Chromatographic separation was performed on a Waters Bridge C18 reversed-phase column (250 x 4.6 mm I.D.; particle size 5 µm), in an isocratic mode with a mobile phase constituted of 90% buffer: 10% acetonitrile (V/V). The buffer was made using 1.5 mL ortho-phosphoric acid, 990 mg 1-Hexanesulfonic acid sodium salt 98%, 140 mg EDTA in 1000 mL flask diluted with HPLC grade water. The elution was carried out at a flow rate of 1.0 mL minˉ1. A diode array detector measured the UV absorbance at 198 nm, in inverse mode. The method was validated for specificity/selectivity, linearity, LOD, LOQ, accuracy, precision and robustness according to ICH validation guidelines. The limits of detection and quantification were calculated at 0.0163 µg/mL and 0.0495 µg/mL, respectively. The method was effectively used for determination of IBN from commercial tablets and provided good results without any interference from commonly used excipients. Keywords: RP-HPLC with indirect UV detection, Ibandronate sodium, validation, pharmaceuticals

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DETERMINATION AND VALIDATION OF MEBHYDROLINE NAPADISYLATE IN TABLETS BY HPLC

Indonesian Journal of Chemistry ◽

10.22146/ijc.21610 ◽

2010 ◽

Vol 8 (3) ◽

pp. 377-379 ◽

Cited By ~ 1

Author(s):

Lestyo Wulandari

Keyword(s):

Quality Control ◽

Ambient Temperature ◽

Mobile Phase ◽

Pharmaceutical Preparation ◽

Reversed Phase ◽

Hplc Method ◽

Uv Detection ◽

Analysis Time ◽

Routine Analysis

An accurate and sensitive HPLC method has been developed for the determination of mebhydroline napadisylate in the tablet. The Chromatography was performed on a reversed phase C-18 column, using a mobile phase of acetonitrile : ammonia 25% (80 : 20 v/v) at ambient temperature 25±5 °C and UV detection operates at 320 nm in an overall analysis time of about 15 min, based on peak area. This HPLC method is selective, precise, and accurate and can be used for routine analysis of pharmaceutical preparation in industrial quality-control laboratories. Keywords : HPLC, mebhydroline napadisylate, validation

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Simultaneous Determination of Preservatives (Methyl Paraben and Propyl Paraben) in Sucralfate Suspension Using High Performance Liquid Chromatography

E-Journal of Chemistry ◽

10.1155/2011/360431 ◽

2011 ◽

Vol 8 (1) ◽

pp. 340-346 ◽

Cited By ~ 5

Author(s):

Rajesh M. Kashid ◽

Santosh G. Singh ◽

Shrawan Singh

Keyword(s):

High Performance Liquid Chromatography ◽

Simultaneous Determination ◽

Mobile Phase ◽

High Performance ◽

Reversed Phase ◽

Hplc Method ◽

Reversed Phase Hplc ◽

Methyl Paraben ◽

Propyl Paraben

A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P.) and propyl paraben (P.P.) is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50) on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precision, specificity, linear range and reproducibility were evaluated. The developed method was applied for the determination of preservative M.P. and P.P. at concentration of 0.01 mg/mL and 0.1 mg/mL respectively. The method was successfully used for determining both compounds in sucralfate suspension.

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VALIDATED RP-HPLC METHOD FOR DETERMINATION OF ENZALUTAMIDE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽

10.53879/id.53.11.10670 ◽

2016 ◽

Vol 53 (11) ◽

pp. 46-50

Author(s):

Z. G Khan ◽

◽

S. S. Patil ◽

P. K. Deshmukh ◽

P. O. Patil

Keyword(s):

Retention Time ◽

Mobile Phase ◽

High Performance ◽

Reversed Phase ◽

Hplc Method ◽

Uv Detector ◽

Chromatography Method ◽

Pharmaceutical Dosage Form ◽

Bulk Drug

Novel, isocratic reversed phase high performance liquid chromatography method was developed and validated for the determination of enzalutamide (EZA) in bulk drug and pharmaceutical formulation. Efficient separation was achieved on PrincetonSPHER C18 100A, 5μ (250×4.6 mm) under the isocratic mode of elution using acetonitrile: water (80:20) % V/V as a mobile phase pumped in to the column at flow rate 1.0 mL/min. The effluent was monitored at 237.0 nm using UV detector. EZA was eluted in the given mobile phase at retention time (tR) of 3.2 minutes. The standard calibration curve was linear over the concentration range 10 - 60 μg/mL with correlation coefficient 0.997. The method was validated for accuracy, precision, sensitivity, robustness, ruggedness and all the resulting data treated statistically. The system suitability parameters like retention time, theoretical plates, tailing factor, capacity factor were found within the limit.

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

Current Chemistry Letters ◽

10.5267/j.ccl.2021.3.001 ◽

2021 ◽

pp. 281-294 ◽

Cited By ~ 1

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.

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Molecular and Quantum Mechanical Study for the Separation of Cefprozil in the Presence of Its Alkaline Degradation Product Using RP-HPLC with UV Detection

Journal of AOAC International ◽

10.5740/jaoacint.16-0246 ◽

2017 ◽

Vol 100 (2) ◽

pp. 392-399 ◽

Cited By ~ 2

Author(s):

Khalid A M Attia ◽

Mohammed W I Nassar ◽

Mohamed B El-Zeiny ◽

Ahmed Serag

Keyword(s):

Degradation Product ◽

Generation Cephalosporin ◽

Reversed Phase ◽

Hplc Method ◽

Uv Detection ◽

Quantum Mechanical ◽

Rp Hplc ◽

Quantum Mechanical Study ◽

Alkaline Conditions

Abstract A reversed-phase HPLC method (RP-HPLC) with UV detection was developed and validated for the quantitative determination of cefprozil, a second-generation cephalosporin. Due to β-lactam ring instability under alkaline conditions, this RP-HPLC method was applied for the determination of cefprozil in the presence of its possible degradation product. The interactions that govern the separation process with stationary phase were investigated at both molecular and quantum mechanical levels. Moreover, electrostatic potential maps were generated to determine the sites of interaction with mobile phase. The suggested method was validated in compliance with International Conference on Harmonization guidelines and successfully applied for the determination of cefprozil in its commercial pharmaceutical formulation.

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Chromatographic Methods for the Determination of Primula Acid 1 Content in Primulae extractum fluidum

Glasnik hemicara i tehnologa Bosne i Hercegovine ◽

10.35666/ghtbh.2020.54.03 ◽

2020 ◽

Keyword(s):

Calibration Curve ◽

Mobile Phase ◽

Active Component ◽

Reversed Phase ◽

Hplc Method ◽

Reversed Phase Chromatography ◽

Triterpenoid Saponins ◽

Simple Preparation ◽

Primula Veris

Primula veris L. (Primulaceae)is healing plant, whose root is officially used to treat cough associated with cold. Other reported indications are respiratory, thoracic and mediastinal disorders. These effects are result of high contents of triterpenoid saponins and phenolic glycosides. Primula acid 1 (PA 1, also primulasaponin 1) is main active component in Primula elatior L. This paper presents an optimized high pressure liquid chromatography (HPLC) method for the determination of primula acid 1 content in Primulae extractum fluidum. TLC was performed to check for the presence of the substance of interest. The determination was performed by reversed phase chromatography using C18 as a stationary phase. The mobile phase used for separation consisted of 0.2% H3PO4 and acetonitrile. This method was validated through different parameters. The detection limit for primula acid 1 was LD=10.41 µg/ml, and the quantification limitwas LQ=34.69 µg/ml. In order to determine the content of primula acid 1, a calibration curve was constructed, and the content of primula acid 1 was calculated by the equation of the calibration curve and was 0.2793 mg per gram of extract. The results and simple preparation of sample show that HPLC is the method of choice for this type of analysis.

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Development and application of a validated HPLC method for the analysis of dissolution samples of mexiletine hydrochloride capsules

Journal of the Serbian Chemical Society ◽

10.2298/jsc090728065m ◽

2010 ◽

Vol 75 (7) ◽

pp. 975-985 ◽

Cited By ~ 1

Author(s):

Dragan Milenovic ◽

Zoran Todorovic

Keyword(s):

Flow Rate ◽

Mobile Phase ◽

Hplc Method ◽

Uv Detection ◽

In Vitro Dissolution ◽

Selective Method ◽

Dissolution Studies ◽

Detection And Quantification

The aim of this work was to develop and validate a simple, efficient, sensitive and selective method for the analysis of dissolution samples of mexiletine hydrochloride capsules by HPLC without the necessity of any time-consuming extraction, dilution or evaporation steps prior to drug assay. Separation was performed isocratically on a 5 ?m LiChrospher 60, RP-Select B column (250 x 4 mm ID) using the mobile phase buffer-acetonitrile (60:42, v/v) at a flow rate of 1.2 mL min-1 and UV detection at 262 nm. The elution occurred in less than 10 minutes. The assay was linear in the concentration range 50-300 ?g mL-1 (r2 = 0.9998). The validation characteristics included accuracy, precision, linearity, specificity, limits of detection and quantification, stability, and robustness. Validation acceptance criteria were met in all cases (the percent recoveries ranged between 100.01 and 101.68 %, RSD < 0.44 %). The method could be used for the determination of mexiletine hydrochloride and for monitoring its concentration in in vitro dissolution studies.

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

Drug Analytical Research ◽

10.22456/2527-2616.79216 ◽

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.

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Ultra-Performance Liquid Chromatographic and Densitometric Methods for Sensitive Determination of Xipamide and Triamterene in Pure and Pharmaceutical Dosage Forms

Journal of AOAC International ◽

10.1093/jaoacint/qsab110 ◽

2021 ◽

Author(s):

N V Fares ◽

Haitham A El Fiky ◽

Amr M Badawey ◽

Maha F Abd El Ghany

Keyword(s):

Acetic Acid ◽

Flow Rate ◽

Mobile Phase ◽

Dosage Forms ◽

Hplc Method ◽

Uv Detection ◽

Pharmaceutical Dosage Forms ◽

Selective Determination ◽

Liquid Chromatographic

Abstract Background Validated UPLC method and TLC densitometric method were prescribed for determination of antihypertensive components. Objectives: To establish and validate rapid and accurate Ultra performance liquid chromatographic (UPLC) and TLC densitometric methods for determination of Xipamide and Triamterene in pure and dosage forms. Methods The first method; UPLC method, depended on using Agilent Zorbax Eclipse Plus C8 (50 mm × 2.1 mm, 1.8 μm), as the column, mobile phase composed of (acetonitrile-water) (70 + 30, v/v) adjusted by acetic acid to obtain (pH 3), 0.2 mL/min flow rate and UV detection at 231.4 nm. The second method was a thin layer chromatography (TLC) densitometric method, separation was achieved by using toluene-methanol-ethyl chloride-acetic acid (7 + 2 + 1 + 0.2, v/v/v) as the mobile phase, pre coated silica gel plates as the stationary phase and UV detection at 300.0 nm. Results The obtained results were validated and statistically compared with official and reported methods. The obtained results showed high accuracy and reproducible results with excellent mean recoveries for both drugs. Conclusions The UPLC method showed shorter retention time for both Xipamide (0.88 min) and Triamterene (0.63 min), lower detection limit less than 0.055 µg/mL for both drugs with high selectivity, decreased injection volume (1 µL) and lower flow rate other than any HPLC method. Both proposed methods were sensitive, selective, and effectively applied to pure and dosage forms (Epitens®). Highlights Unprecedented sensitive, rapid, and reproducible UPLC and TLC methods were developed for selective determination of mixture of Xipamide and Triamterene with LOD less than 0.076 µg/mL for both drugs.

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