scholarly journals Development and Validation of Novel RP-HPLC Method for the Simultaneous Determination of Remogliflozin and Vildagliptin in Bulk and in synthetic Mixture

2021 ◽  
pp. 338-349
Author(s):  
Drashti A. Mandale ◽  
Chainesh Shah ◽  
Rakesh Jatt
Keyword(s):  
Single Dose ◽  
Dose Regimen ◽  
High Performance ◽  
Sglt2 Inhibitor ◽  
Hplc Method ◽  
Synthetic Mixture ◽  
Chromatography Method ◽  
Drug Sample ◽  
Liquid Chromatography Method

Vildagliptin which is DPP-4 inhibitor and Remogliflozin which is SGLT2 inhibitor in single dose regimen lower blood glucose by separate, complementary mechanisms. Both are glucose dependent, accounting for the low risk of hypoglycaemia during treatment. There is no risk factors associated with this combination and moreover it is single dose regimen. The aim of the present study was to develop and validate a simple, rapid and reproducible gradient high performance reverse phase liquid chromatography method for the estimation of Remogliflozin and Vildagliptin in bulk drug sample and in synthetic mixture using Xterra® Waters C18 column (150 mm×4.6 mm, 5 µm) at 25°C with UV detection at 210 nm and for this gradient mode was used. The compounds were eluted gradiently at a flow rate of 1.0ml/min. The average retention times for Remogliflozin and Vildagliptin were 4.881 and 6.334 min, respectively. The calibration curves were linear (r2 =0.988) over the concentration range 10-200 µg/ml for Remogliflozin and 10-200 µg/ml for Vildagliptin. No spectral or chromatographic interferences from formulation excipients were found and hence it was successfully applied for the determination of Remogliflozin and Vildagliptin in bulk and in synthetic mixture. The accuracy of the proposed method was determined by recovery studies and found to be 98-101%. The proposed method was validated and results conformed to ICH parameters.

scholarly journals Quantitative Estimation of Sorafenib Tosylate Its Pure Form and in Its Tablet Formulation by RP-HPLC Method

2013 ◽  
Vol 2013 ◽  
pp. 1-3 ◽  
Author(s):  
R. Kalaichelvi ◽  
E. Jayachandran
Keyword(s):  
High Performance ◽  
Quantitative Estimation ◽  
Hplc Method ◽  
Pure Form ◽  
Mobile Phase Composition ◽  
Chromatography Method ◽  
Rp Hplc ◽  
Liquid Chromatography Method ◽  
Isocratic Mode

A simple, accurate, specific reverse-phase, high-performance liquid chromatography method has been developed for the determination of sorafenib tosylate in its pure form and its tablets. In this method, sorafenib tosylate was eluted by isocratic mode using a Phenomenex Luna C18 column by a mobile phase composition of acetonitrile and water in the ratio of 82.5 : 17.5, v/v. The flow rate was 1.5 mL/min. The eluted drug was monitored at 265 nm and the method was found to be linear from 5 to 80 μg/mL. The method was validated by linearity, precision, accuracy, LOD, and LOQ. The accuracy report denotes that there is not any interference of additives used in the formulation.

Development of a sulphurous acid thiolysis-high performance liquid chromatography method for the analysis of procyanidins in pine bark products

2020 ◽  
Vol 10 (9) ◽  
pp. 1581-1587
Author(s):  
Lei Shi ◽  
Chunqi Liang ◽  
Yongzhi Qi
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Hplc Method ◽  
Pine Bark ◽  
Epicatechin Gallate ◽  
Chromatography Method ◽  
Content Determination ◽  
Liquid Chromatography Method

A sulphurous acid thiolysis-HPLC method for the determination of procyanidins in pine bark products was established. The concentration of sulphurous acid is 1.2%, the concentration of benzyl mercaptan is 2%, the reaction temperature is 90 °C, and the reaction time is 60 minutes. Under these conditions, the preservative rates of catechin, epicatechin, epicatechin gallate and their benzyl sulfide derivatives were 89.7%, 86.2%, 95.4%, 63.1%, 64.6% and 73.5%, respectively. According to this study, the calculation method for the procyanidin content determination by the thiolysis-HPLC method was corrected.

RAPID HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF RALTEGRAVIR IN HUMAN SALIVA

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (09) ◽  
pp. 68-73
Author(s):  
K Vijaya Sri ◽  
M. Shiva Kumar ◽  
M. A. Madhuri ◽  
Suresha K. ◽  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Human Saliva ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
Liquid Chromatographic

In this study, a high-performance liquid chromatographic method (HPLC) was developed, validated and applied for the determination of raltegravir in biological sample like saliva. Liquid- liquid extraction was performed for isolation of the drug and elimination of saliva interferences. Samples of saliva was extracted with 50µL of ortho phosphoric acid and 3ml of methanol was added and spiked with raltegravir. The chromatographic separation was performed on Agilent Eclipse C18 (100 mm × 4.6 mm, 3.5µm) column, by using 80:20 v/v acetonitrile: water as a mobile phase under isocratic conditions at a flow rate of 1.0 mL/min for UV detection at 240 nm. Retention time of raltegravir was found to be 1.030 min. Linearity was found to be in the range of 25-1000 ng/mL with regression equation y = 13864x + 40495 and correlation coefficient 0.999. The low % RSD value indicates the method is accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.76 and 2.28 ng/mL, respectively. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for determination of raltegravir in saliva.

Development and Validation of a High-performance Liquid Chromatography Method with Ultraviolet Detection for the Determination of Flunitrazepam in Human Plasma

2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Bela Kiss ◽  
Daniela-Saveta Popa ◽  
Marius Bojita ◽  
Felicia Loghin
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Hplc Method ◽  
Simple Liquid ◽  
Chromatography Method ◽  
Liquid Chromatography Method ◽  
The Stability

A high performance liquid chromatography (HPLC) method was developed and validated for determination of flunitrazepam in human plasma. After a simple liquid-liquid extraction, the analyses were carried out on a ODS column with diode array detection at 330nm. The mobile phase consisted in a mixture of potassium dihydrogene phosphate/acetonitrile (40/60, v/v). The method showed good linearity, accuracy and precision. Advantages of this validated assay include a simple plasma extraction method, short analysis time and good sensitivity (LLOQ = 5ng/mL). The stability data indicated a potential instability of flunitrazepam in plasma at room temperature.

scholarly journals Development and Validation of Rapid and Sensitive HPLC Method for the Determination of Methotrexate in Human Serum

2010 ◽  
Vol 2 (1) ◽  
pp. 8-13 ◽  
Author(s):  
M Nagulu ◽  
V Uday Kiran ◽  
Y Narsimha Reddy ◽  
D Rama Krishna
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Hplc Method ◽  
High Dose ◽  
Chromatography Method ◽  
Quantitation Limit ◽  
High Doses ◽  
Liquid Chromatography Method ◽  
Development And Validation

Methotrexate competitively inhibits dihydrofolic acid reductase and thereby inhibits DNA synthesis and cellular replication.This study describes a simple and fast high-performance liquid chromatography method for the determination of methotrexate [MTX] in serum.samples were collected from adult cancer patients receiving high dose MTX at Mahathma Gandhi Memorial hospital (Warangal,AP.India) at various time intervals after the end of each infusion. Serum was deproteinized with trichloroacetic acid and the supernatant was injected into a 250×4.6 mm octadecylsilane column. Mobile phase was made of TRIS-phosphate buffer (pH 5.7): methanol: acetonitrile (70:20:10) with a flow rate of 1ml/min. Ultraviolet detection was done at 313 nm and at ambient temperature. Para aminoacetophenone was used as internal standard. Methotrexate and internal standard retention times were 4.6 and 9.5 minutes, respectively. Results showed that reproducibility (precision) of method within a day was 2.6 to 6 percent and between days was 5.5 to 9.5 percent. The recovery of the method was between 61.5 and 72.7 percent. The quantitation limit of the method for methotrexate was 0.1μM. This method is suitable for quantitation of methotrexate after infusion of high doses of this drug and has good accuracy, precision and quantitation limit. Key Words: Methotrexate; HPLC; Serum Concentration. DOI: 10.3329/sjps.v2i1.1693Stamford Journal of Pharmaceutical Sciences Vol.2(1) 2009: 8-13

scholarly journals DEVELOPMENT OF METHODS FOR DETERMINATION OF SPECIFIC IMPURITIES IN THE GLUTATIONION RESTORED SUBSTANCE

2019 ◽  
Vol 6 (6) ◽  
pp. 535-547
Author(s):  
K. A. Alexeeva ◽  
D. I. Pisarev ◽  
A. Yu. Malyutina ◽  
N. N. Boyko
Keyword(s):  
Amino Acids ◽  
High Performance ◽  
Hplc Method ◽  
Low Molecular Weight ◽  
Chromatography Method ◽  
Rp Hplc ◽  
Liquid Chromatography Method ◽  
Layer Chromatography ◽  
Better Than

Glutathione (γ-L-glutamyl-L-cysteinylglycine) is the most important low molecular weight intracellular thiol tripeptide consisting of three amino acids – glycine, cysteine and glutamic acid. In Russian pharmacopoeia there is no regulatory documentation for glutathione, therefore, the development of a pharmacopoeial item for the specified substance is a relevant problem.The aim of the article is the development of methods for determining foreign specific impurities in glutathione.Materials and methods. The substance of glutathione reduced (CAS 70-18-8, EC 2007254, Applichem, Germany) containing impurities, and a standard sample of reduced glutathione (Sigma Aldrich, Japan) were used as the objects of the study. The analysis was carried out by using a high-performance liquid chromatography method in the reverse phase version and a thin layer chromatography method. The chromatography using RP HPLC was performed after preliminary derivatization of glutathione and its specific impurities with dancil chloride. Specific impurities in glutathione are dipeptides and amino acids. Therefore, they, like glutathione, can react with dancil chloride. Dancil derivatives are formed, and they can be determined by chromatographic separation.Results. As a result of chromatography by the method of RP HPLC of derivatized dancil chloride glutathione it has been established that this reaction makes it possible to detect impurities in it. Glutathione derivatives are well separated by chromatography by implementing the method of RP HPLC and have different absorption maxima. The glutathione derivative had an absorption maximum at λmax=284 nm. The derivatives belonging to specific glutathione impurities absorb at λmax=288 nm and λmax=296 nm. The data obtained using RP HPLC were confirmed by TLC in the isopropanol-water (2:1) system. Three components were found out, one of which corresponds to glutathione, while two others are impurities.Conclusion. Methods for determining impurities in the glutathione substance using RP HPLC methods with preliminary derivatization with dancil chloride and TLC with ninhydrin detection have been worked out. A comparative analysis of the data obtained makes it possible to state that the OF-HPLC method with pre-column derivatization is more reliable, since it is more sensitive to impurities, and also makes it possible to study the UV profiles of impurity components better than the TLC method. Therefore, for the detection of impurities in the substance of glutathione, it is more preferable to use RP-HPLC with pre-column derivatization. The results of this study can be recommended for inclusion in the regulatory documentation on the substance of glutathione in the section “Impurities”.

scholarly journals Development and Validation of a Column High-Performance Liquid Chromatography Method for Quantification of Ganaphaliin A and B in Inflorescences of Gnaphalium liebmannii Sch. Bp ex Klatt

2011 ◽  
Vol 94 (4) ◽  
pp. 1076-1081 ◽  
Author(s):  
Fernando Rodríguez-Ramos ◽  
Víctor H Sánchez-Estrada ◽  
Alejandro Alfaro-Romero ◽  
Gabriela Rubí Tapia-Álvarez ◽  
Andrés Navarrete
Keyword(s):  
High Performance ◽  
Hplc Method ◽  
Raw Material ◽  
Array Detector ◽  
Chromatography Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Liquid Chromatography Method ◽  
Development And Validation

Abstract An HPLC method was developed for the simultaneous determination of gnaphaliin A and B, active compounds of Gnaphalium liebmannii Sch. Bp ex Klatt. The HPLC separation was performed on an Inertsil ODS-3 (150 × 4.6 mm id, 5 μm) RP C18 column operated at 40°C; the isocratic mobile phase was 0.02% aqueous orthophosphoric acid– methanol–acetonitrile (50 + 30 + 20, v/v/v), with a run time of 20 min and flow rate of 1.5 mL/min. Detection with a photodiode array detector (PDAD) was at 270 nm. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ for gnaphaliin A and B were found to be in the range of 0.4–0.5 and 1.0–1.4 μg/mL, respectively. This is the frst report of an analytical method developed for the quantitative analysis of flavones from Gnaphalium species by HPLC-PDAD with applications for raw material and commercial products.

HPLC DETERMINATION OF N-METHYLETHANOLAMINE IN DIPHENHYDRAMINE HYDROCHLORIDE DRUG SUBSTANCE BY PRE-COLUMN DERIVATIZATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (10) ◽  
pp. 56-62
Author(s):  
A Anerao ◽  
◽  
V. Dighe ◽  
A Gupta ◽  
C. Patil ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Diphenhydramine Hydrochloride ◽  
Liquid Chromatography Method

N-Methylethanolamine is the side chain of the drug diphenhydramine hydrochloride. A sensitive high performance liquid chromatography method with pre-column derivatization was developed and validated for the determination of N-methylethanolamine impurity in diphenhydramine hydrochloride active pharmaceutical ingredient. HPLC method on column Cosmosil MS-II, C-18, 250 mm X 4.6 mm, particle size 5 μm with UV detector was used. The proposed method is specific, linear, accurate, rugged and precise. The calibration curves showed good linearity over the concentration range of 0.03 mg/g to 1.5 mg/g and the correlation coefficient was 0.999. Method had very low limit of detection (LOD) and limit of quantification (LOQ) as 0.01 mg/g and 0.03 mg/g, respectively, of the analyte. Accuracy was observed within 94.4% to 96.2%.

Developing a High-Performance Liquid Chromatography (HPLC) Method for Simultaneous Determination of Oxytetracycline, Tinidazole and Esomeprazole in Human Plasma

2019 ◽  
Vol 57 (8) ◽  
pp. 724-729 ◽  
Author(s):  
Mahmoud M Sebaiy ◽  
Wafaa S Hassan ◽  
Mostafa E Elhennawy
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
High Performance ◽  
Hplc Method ◽  
Chromatography Method ◽  
Simultaneous Separation ◽  
Liquid Chromatography Method ◽  
High Degree

Abstract A high performance liquid chromatography method had been developed and validated for rapid simultaneous separation and determination of three anti-helicobacter drugs, oxytetracycline (OXY), tinidazole (TIN) and esomeprazole (ESM) in human plasma within 6 minutes. Drugs extraction method from plasma was based on protein precipitation technique. Separation was carried out on a Equisil BDS C18 column (5 μm, 150 × 4.60 mm) using a mobile phase of acetonitrile: 0.025 M KH2PO4 (25: 75, v/v) adjusted to pH 3.50 with ortho-phosphoric acid at ambient temperature. The flow rate was 1 mL/min and maximum absorption was measured using Diode Array (DAD) detector at 285 nm. The retention times of OXY, TIN and ESM were recorded to be 2.68, 3.52 and 5.17 minutes, respectively, indicating a shorter analysis time. Limits of detection were also reported to be 0.10, 0.07 and 0.04 μg/mL for OXY, TIN and ESM, respectively, showing a high degree of the method sensitivity. The method was then validated according to FDA guidelines for the determination of the drugs clinically in human plasma specially regarding pharmacokinetic and bioequivalence studies.

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