scholarly journals ANALYITCAL METHOD DEVELOPMENT AND VALIDATION OF A REVERSED-PHASE HIGHPERFORMANCE LIQUID CHROMATOGRAPHY FOR THE DETERMINATION OF MODAFINIL IN BULK AND PHARMACEUTICAL DOSAGE FORMS

2016 ◽  
Vol 9 (5) ◽  
pp. 177
Author(s):  
Bijithra Cholaraja ◽  
Shanmugasundaram P ◽  
Ragan G ◽  
Sankar Ask ◽  
Sumithra M
Keyword(s):  
Particle Size ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Rp Hplc ◽  
Development And Validation

ABSTRACTObjective: To development and validation of a reversed-phase high-performance liquid chromatography (RP-HPLC) for the determination of modafinilin bulk and pharmaceutical dosage forms.Methods: A simple, precise, rapid, and accurate RP-HPLC method was developed for the estimation of modafinil in bulk and pharmaceutical dosageforms. Xterra RP 18 (250 mm × 4.6 mm, 5 µ particle size) with a mobile phase consisting of methanol:water 70:30 V/V was used. The flow rate1.0 ml/min and the effluents were monitored at 260 nm. The retention time and recovery time was 12 minutes. The detector response was linear inthe concentration of 10-50 µg/ml. The respective linear regression equation being Y=452.1x+65237. The limit of detection and limit of quantificationwere 4.547 and 1.377 mcg, respectively. The method was validated by determining its accuracy, precision, and system suitability.Result: The objective of the present work is to develop simple, precise, and reliable HPLC method for the analysis of modafinil in bulk andpharmaceutical dosage forms. This is achieved using the most commonly employed Xterra RP 18 (250 mm × 4.6 mm, 5 μ particle size) columndetection at 260 nm. The present method was validated according to ICH guidelines.Conclusion: In this study, a simple, fast and reliable HPLC method was developed and validated for the determination of modafinil in pharmaceuticalformulations.Keywords: Modafinil, Reversed-phase high-performance liquid chromatography, Estimation, ICH guidelines, Tablets. 

Development and Validation of a RP-HPLC Method for the Simultaneous Determination of LevamisoleHCl and Oxyclozanideand its Application in the Assay of Veterinary Bolus Formulations

2020 ◽  
Vol 16 ◽  
Author(s):  
Kemal Hussien Seid ◽  
Tarekegn Berhanu ◽  
Kaleab Asres ◽  
Ayenew Ashenef
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Average Accuracy ◽  
Development And Validation

Introduction: A reverse-phase high performance liquid chromatography (RP-HPLC) method was developed and validated for the simultaneous analysis of two drugs, levamisole hydrochloride(LH) and oxyclozanide(OX), in co-formulations for veterinary use. Materials and Methods: The new HPLC method was validated per ICH and other guidelines. A C18 column was used with agradient program; eluent A was an equal mixture of methanol and acetonitrile, and eluent B a 25 mM phosphate buffer at pH 7.0 containing 30 mM sodium decanesulfonate andtriethylamine(50:50:1 v/v)then pH adjusted to 7.0 with H3PO4 [51:49 v/v] .The detection wavelength was set at 220 nm.For the final gradient program, the retention times were 8.2(for LH)and 13.6(for OX) minutes respectively at flow rate of 1 ml/min over 20 minute run time. Results: The method wasprecise, specific and robust.The correlation coefficients, R2 were 0.9998 and 0.9999 for LH and OX respectively in the ranges of 5 – 280 µg / mL.The percent y-intercepts and percent residual standard deviations were 1.6%/0.4% and 1.4%/1.0% for LH and OX, respectively. The LOD and LOQ of the method were 0.21 µg / mL and 0.62 µg / mL for LHand 0.06 µg / mL and 0.18 µg / mL for OX. The method has average accuracy of 100.5% for LH and 101.1% for OX when tested on veterinary bolus formulations, and the samples couldbe stored under typical lab conditions for about 7 days without significant degradation. Conclusion: This HPLC method is suitable forassayinglevamisole hydrochloride and oxyclozanide simultaneously from veterinary formulations.

Developing a High-performance Liquid Chromatography Method for Simultaneous Determination of Loratadine and its Metabolite Desloratadine in Human Plasma

2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Allergic Diseases ◽  
Reversed Phase ◽  
Hplc Method ◽  
H1 Receptor ◽  
Chromatography Method

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.

Development of reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of selected antihypertensive active flavonoids (rutin, myricetin, quercetin, and kaempferol) in medicinal plants found in Botswana

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Katso Binang ◽  
David T. Takuwa
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Medicinal Plants ◽  
High Performance ◽  
Zingiber Officinale ◽  
Hplc Method ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Lippia Javanica

Abstract The aim of the study was to develop a rapid, efficient, and cheap chromatographic method for determining four selected antihypertensive active flavonoid compounds in medicinal plants in Botswana. The determination of rutin, quercetin, and kaempferol in selected medicinal plants was conducted in less than 6 min using the developed reverse phase-high performance liquid chromatography (RP-HPLC) method with a 2.7 µm Ascentis C18 express column (150 × 4.60 mm i.d) at 340, 360, and 368 nm detection wavelengths and mobile phase of methanol and 0.068% of formic acid solution in isocratic elution. Validation results showed good selectivity, linearity (r 2 > 0.99), high percentage recoveries (90.2–104.7%), and precision (% RSD < 2) for n = 3, confirming suitability of the method for determination of the investigated flavonoids in Zingiber officinale (ginger). Application of the developed RP-HPLC method was performed in selected medicinal plants (Lippia javanica ) (mosukujane), Myrothanmus flabellious (galalatshwene), and Elephantorrhiza elephantina (mositsana) used to manage hypertension by herbalists in Botswana. M. flabellious a very commonly used plant for managing hypertension was found to contain highest amounts of rutin and myricetin, whereas nothing was detected for E. elephantina.

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

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.

Development of a Method for the Determination of Pyrimethamine Concentrations in Feeds by Ion-Pairing High-Performance Liquid Chromatography

2002 ◽  
Vol 65 (4) ◽  
pp. 688-691 ◽  
Author(s):  
P. S. GONG ◽  
S. L. JENG ◽  
Y. F. HSU ◽  
C. C. LIN ◽  
S. Y. LIN
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Ion Pairing ◽  
Reversed Phase ◽  
Hplc Method ◽  
Alumina Column ◽  
Tetramethylammonium Chloride ◽  
Array Detection

An ion-pairing reversed-phase high-performance liquid chromatography (HPLC) method with diode array detection at 280 nm was developed to determine pyrimethamine concentrations in feed for laying hens. Pyrimethamine was extracted with a mixture of 5% isobutanol and 95% benzene, and the extract was cleaned up on an alumina column. The drug was eluted from an Intersil ODS-3V column (250 by 4.6 mm) with a mixture of 25% acetonitrile and 75% water (vol/vol) containing 0.01 M tetramethylammonium chloride as an ion-pairing agent and adjusted with acetic acid to pH 3.5. The flow rate was 1.0 ml/min. Mean recovery of pyrimethamine from supplemented feeds at concentrations of 2, 4, and 5 μg/g of feed were 100.5, 103.5, and 100.8%, respectively. Precision within a day ranged from 4.3 to 7.0% for the three concentrations, and day-to-day precision was 5.3% for feed supplemented at a concentration of 4 μg/g. No chromatographic interference was detected from other 2,4-diaminopyrimidine compounds or other major drugs used in poultry.

Sign in / Sign up

Export Citation Format

Share Document