scholarly journals A Validated RP-HPLC Method for the Determination of Butamirate Citrate and Benzoic Acid in Syrup, Based on an Experimental Design Assessment of Robustness

Separations ◽  
2021 ◽  
Vol 8 (10) ◽  
pp. 163
Author(s):  
Antonios-Dionysios G. Neofotistos ◽  
Kostas Gkountanas ◽  
Haris Boutsikaris ◽  
Yannis Dotsikas
Keyword(s):  
Experimental Design ◽  
Benzoic Acid ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Buffer Solution ◽  
Solution Ph ◽  
Design Assessment ◽  
Rp Hplc

A reversed-phase high-pressure liquid chromatography (RP-HPLC) method was developed and subsequently validated for the simultaneous determination of butamirate citrate (BC) and benzoic acid (BA) in cough syrup. The separation was performed employing a cyanopropyl column with a mobile phase consisting of 50%/50% v/v MeOH/NaH2PO4 * H2O 50 mM aqueous solution pH = 3.0. The quantitation was achieved with a diode array detector (DAD) at 210 nm. The method demonstrated a congenitally satisfactory separation, yet the acquired peaks were asymmetrical. This effect was eliminated by using 1% triethylamine in the buffer solution as a silanol blocker. In addition, the method was found to unequivocally assess the target analytes in the sample matrix and fulfilled the required specifications in relevance to specificity, linearity, accuracy, precision and stability of both the standard solutions and of the sample solutions. Lastly, an experimental design was designed in order to assess the robustness of the proposed assay. To this purpose, a graphical and a statistical approach were utilized and compared to identify the factors that should be strictly controlled during each execution of the method.

scholarly journals Experimental design approach for the development and validation of an enantiospecific RP-HPLC method for simultaneous determination of clopidogrel and related compounds

2008 ◽  
Vol 27 (1) ◽  
pp. 53 ◽  
Author(s):  
Rumenka Petkovska ◽  
Claus Cornett ◽  
Aneta Dimitrovska
Keyword(s):  
Experimental Design ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
Hplc Method ◽  
System Response ◽  
Buffer Solution ◽  
Column Temperature ◽  
Rp Hplc ◽  
Related Compounds

An enantiospecific RP-HPLC method was developed and validated for the simultaneous determination of clopidogrel and four related compounds specified as impurities. Experimental design was applied during the method optimization (Full factorial 23 design) and robustness testing (Central Composite Face Centered design). Laboratory mixtures of clopidogrel and its impurities in a concentration ratio of 1: 5.0×10–4 were used as an investigation matrix. The three independent variables were the acetonitrile content in the mobile phase, pH of the mobile phase, and the column temperature. A Chromatographic Response Function (CRF) was used for estimation of the system response resolution (Rs). Separation was achieved using mobile phase composition of ACN: Buffer solution pH 6.5 (40:60 v/v) at 30 ºC. A CHIRAL-AGP 4.0 mm × 100 mm, 5.0 μm particle size column was used. The total time for chromatographic separation was approximately 10.0 min. The method was validated for its selectivity, linearity, precision, accuracy and robustness.

scholarly journals A Validated Reversed-Phase HPLC Method for the Determination of Vildagliptin from Tablet Dosage Form

2013 ◽  
Vol 2 (3) ◽  
pp. 90-98 ◽  
Author(s):  
Rahima Khatun ◽  
Md Mirazzunnabi
Keyword(s):  
Dosage Form ◽  
Theoretical Plate ◽  
Cost Effective ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Buffer Solution ◽  
Column Temperature ◽  
Tablet Dosage

A simple, rapid, precise and cost effective method has been developed and validated for determination of Vildagliptin in pharmaceutical tablet dosage form. The chromatographic separation was carried out with Shimpack VP-ODS, 150 × 4.6 mm, 5?m analytical column and mobile phase containing 0.02M phosphate buffer (pH 4.6) and acetonitrile at the ratio (80:20% v/v). pH of the buffer solution was adjusted with orthophosphoric acid. The instrumental settings include flow rate 0.7 ml/min, column temperature at 25ºC and detector wavelength of 210nm using a photodiode array detector. Theoretical plate for Vildagliptin was 6219 and tailing factor was 1.38. DOI: http://dx.doi.org/10.3329/ijpls.v2i3.15455 International Journal of Pharmaceutical and Life Sciences Vol.2(3) 2013: 90-98

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

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

scholarly journals Development and Validation of Stability Indicating RP-HPLC Method for Estimation of Satranidazole from Its Formulation

2014 ◽  
Vol 2014 ◽  
pp. 1-7
Author(s):  
Harshal Ashok Pawar ◽  
Pooja Rasiklal Joshi
Keyword(s):  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Solution Ph ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Eudragit E100 ◽  
Development And Validation

Satranidazole is a new nitroimidazole derivative with potent antiamoebic action and is available in market in the form of tablet and dry syrup either alone or in combination with Ofloxacin. The present study involves the development of simple, accurate, precise, and reproducible reversed phase high performance liquid chromatography (RP-HPLC) method for determination of Satranidazole from its granular dosage form. Isocratic elution at a flow rate of 1.0 mL/min was employed on BDS Hypersil C18 (250 mm × 4.6 mm, 5 μm) column at 25°C temperature. The mobile phase consists of 0.16% v/v orthophosphoric acid solution, pH 3: acetonitrile in the ratio of 60 : 40 v/v. The UV detection wavelength was 320 nm, and 20 μL sample was injected. The retention time for Satranidazole was about 4.3 minutes. The method was validated for various parameters such as system suitability, precision, recovery, robustness, and ruggedness as per ICH guidelines. The validated RP-HPLC method was found to be specific, linear, precise, and accurate and can be successfully employed for the assay of Satranidazole taste masked granules coated with Eudragit E100 and marketed tablets.

Development and validation of a fast and simple HPLC method for the simultaneous determination of aniline and its degradation products in wastewater

2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Simple Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Development And Validation

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.

scholarly journals Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

2012 ◽  
Vol 48 (2) ◽  
pp. 315-323 ◽  
Author(s):  
Paulo Cesar Pires Rosa ◽  
Isabel Cristina Sales Fontes Jardim
Keyword(s):  
Stationary Phase ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Polar Groups ◽  
Ich Guidelines ◽  
Relative Standard ◽  
New Stationary Phase

A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO) and doxylamine succinate (DOX) in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size) synthetized at the Liquid Chomatography Laboratory (LabCrom) of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5) in the gradient mode. The diode array detector (DAD) was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD) less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX) over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX). The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.

QBD BASED RP-HPLC METHOD FOR SCREENING AND ANALYSIS OF TELAPRAVIR AND 7 OTHER ANTIRETROVIRAL AGENTS

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (02) ◽  
pp. 20-33
Author(s):  
N. S Kumar ◽  
◽  
R Kumaraswamy ◽  
S. Shantikumar ◽  
D. Paul
Keyword(s):  
Quality By Design ◽  
Pharmaceutical Formulations ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Array Detector ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Full Factorial

The present study describes the separation and simultaneous estimation of eight anti-retroviral drugs, namely, Telaprevir (TPV), Emtricitabine (ECB), Fosamprenavir (FANV), Tenofavir (TNF), Ritonavir (RNV), Raltegravir (RGV) and Oseltamivir (OSMV) and Zidovudine (ZDV) as an active pharmaceutical ingredient, by RP-HPLC method by applying the principles of Quality by Design (QbD). An application of DoE (Design of Experiments) full factorial design was used for initial screening and optimization. The final optimized method consists of separation being carried out on a Fortis C18 column (150 mm × 4.6 mm, 5μ particle size) using acetonitrile and 10 mm ammonium formate buffer (pH 3 adjusted with formic acid) using a gradient program. The quantitative evaluation was performed with a diode array detector at 251 nm and 230 nm with a flow rate of 1 mL min–1. Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with the International Conference on Harmonization (ICH) guidelines. The method is selective, precise, robust and accurate and can be used for routine analysis of pharmaceutical formulations in quality control and counterfeit screening.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF β-ACETYLDIGOXIN

2016 ◽  
Vol 9 (1) ◽  
pp. 54
Author(s):  
Megha Sharma ◽  
Neeraj Mahindroo
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Hplc Method ◽  
Stability Study ◽  
Array Detector ◽  
Forced Degradation ◽  
Simple Method ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The objective of the present study was to develop and validate a novel stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of β-acetyldigoxin, an active pharmaceutical ingredient (API).Methods: The chromatographic separation was carried out on Agilent Technologies 1200 series HPLC system equipped with photo diode array detector and C-18 (4.6x250 mm, 5 µ) column. The mobile phase consisted of water: acetonitrile (65:35 v/v), delivered at a flow rate of 1.5 ml/min and eluents were monitored at 225 nm.Results: The retention time of β-acetyldigoxin was 9.2 min. The method was found to be linear (R2= 0.9995) in the range of 31.25-500 µg/ml. The accuracy studies showed the mean percent recovery of 101.02%. LOD and LOQ were observed to be 0.289 µg/ml and 0.965 µg/ml, respectively. The method was found to be robust and system suitability testing was also performed. Forced degradation analysis was carried out under acidic, alkaline, oxidative and photolytic stress conditions. Significant degradation was observed under tested conditions, except for oxidative condition. The method was able to separate all the degradation products within runtime of 20 min and was able to determine β-acetyldigoxin unequivocally in presence of degradation products.Conclusion: The novel, economic, rapid and simple method for analysis of β-acetyldigoxin is reported. The developed method is suitable for routine quality control and its determination as API, and in pharmaceutical formulations and stability study samples.

Ecofriendly chromatographic methods for determination of co-prescribed drugs, olanzapine and metformin, in rat plasma

Bioanalysis ◽  
2020 ◽  
Vol 12 (9) ◽  
pp. 597-613
Author(s):  
Aml A Emam ◽  
Neven M Habib ◽  
Hamada M Mahmoud ◽  
Nada S Abdelwhab ◽  
Maha M Abdelrahman
Keyword(s):  
Pharmaceutical Preparation ◽  
Rat Plasma ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hypoglycemic Agent ◽  
Chromatographic Methods ◽  
Rp Hplc ◽  
Development And Validation ◽  
Developing System

Background: Olanzapine (OLZ) is one of most recommended drugs for the treatment of schizophrenia while metformin (MET) is the most commonly used hypoglycemic agent. Aim: Development and validation of two green, sensitive and accurate chromatographic methods for the simultaneous determination of OLZ along with the co-prescribed, MET. Materials & methods: TLC-densitometric method with a developing system consisting of methylene chloride:methanol:ethyl acetate:triethylamine (4:4:5:0.1, by volume) and a reversed-phase (RP)-HPLC method where the chromatographic separation was performed using ethanol:water mixture (50: 50, v/v) as a mobile phase. Results: TLC-densitometric method had linearity over concentration ranges of 160–4000 ng/band for OLZ and 150–4500 ng/band for MET, while RP-HPLC method was linear and validated over concentration range of 300–20000 ng/ml for OLZ and MET. Conclusion: Pharmacokinetic study was successfully performed and suggested the possibility of co-administration of MET with OLZ and their further formulation in one pharmaceutical preparation to enhance patient’s compliance.

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