scholarly journals Development and Validation of Stability-Indicating RP-HPLC Method for Simultaneous Determination of Metformin HCI and Glimepiride in Fixed-Dose Combination

2016 ◽  
Vol 11 ◽  
pp. ACI.S38137 ◽  
Author(s):  
Pradnya N. Vaingankar ◽  
Purnima D. Amin
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Fixed Dose ◽  
Metformin Hydrochloride ◽  
Chromatography Method ◽  
Stress Degradation ◽  
Degradation Studies

A simple reversed-phase high-performance liquid chromatography method was developed and validated for simultaneous determination of Metformin hydrochloride (MET) and Glimepiride (GLM) in combination and estimation of their principal degradation products. The separation was achieved using JASCO Finepak SIL (250 mm × 4.6 mm i.d. 5 μm) at ambient temperature. The optimized mobile phase composed of an aqueous phase (20 mM phosphate buffer, adjusted to pH 3.0) and an organic phase (methanoliacetonitrile; 62.5:37.5) in the ratio of 80:20. The flow rate was 1 mL/minute, and the analytes were detected at 230 nm. The developed method was validated for accuracy, precision, specificity, linearity, and sensitivity. The chromatographic analysis time was approximately six minutes with the complete resolution of MET (Rt = 2.75 minutes) and GLM (Rt = 5.87 minutes). The method exhibited good linearity over the range of 5-30 μg/mL for MET and 1-10 μg/mL for GLM. The drugs in combination were subjected to various stress degradation studies as per the International Conference Harmonization (ICH) guidelines. Results obtained from the stress degradation studies revealed that the developed method is applicable for stability studies.

scholarly journals Simple and rapid liquid chromatography method for simultaneous determination of isoniazid and pyrazinamide in plasma

2012 ◽  
Vol 9 (1) ◽  
pp. 13-18 ◽  
Author(s):  
AK Kumar Hemanth ◽  
V Sudha ◽  
G Ramachandran
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Small Sample Size ◽  
Accurate Method ◽  
Reversed Phase ◽  
Small Sample ◽  
Pharmacokinetic Studies ◽  
Chromatography Method ◽  
Relative Standard

Introduction: Treatment of tuberculosis (TB) requires a combination of drugs. Isoniazid (INH) and pyrazinamide (PZA) are key components of the fi rst-line regimen used in the treatment of TB and monitoring these drug levels in plasma would help in better patient care. The objective of the study is to develop and validate a simple and rapid high performance liquid chromatographic method for simultaneous determination of INH and PZA in human plasma. Methodology: The method involved deproteinisation of plasma with para hydroxy benzaldehyde and trifl uoroacetic acid and analysis using a reversed-phase C8 column and UV detection at 267nm. The fl ow rate was set at 1.5 ml/min at ambient temperature. The accuracy, linearity, precision, specifi city, stability and recovery of the method were evaluated. The method was applied to estimate plasma INH and PZA collected from six children with TB. Results: Well resolved peaks of PZA and INH at retention times of 3.2 and 6.1 minutes respectively were obtained. The assay was linear from 0.25 - 10.0 ìg/ml for INH and 1.25 – 50.0 ìg/ml for PZA. The within-day and between-day relative standard deviation for standards were below 10%. The average recoveries of INH and PZA from plasma were 104 and 102% respectively. Conclusions: A rapid and accurate method for simultaneous determination of INH and PZA in plasma was validated. The assay spans the concentration range of clinical interest. The easy sample preparation and small sample size makes this assay highly suitable for pharmacokinetic studies of INH and PZA in TB patients. SAARC Journal of Tuberculosis, Lung Diseases & HIV/AIDS 2012; IX (1) 13-18 DOI: http://dx.doi.org/10.3126/saarctb.v9i1.6960

Stability-Indicating RP-HPLC and CE Methods for Simultaneous Determination of Bisoprolol and Perindopril in Pharmaceutical Formulation: A Comparative Study

2020 ◽  
Vol 58 (8) ◽  
pp. 747-758
Author(s):  
Said A Hassan ◽  
Nancy W Nashat ◽  
Mohamed R Elghobashy ◽  
Samah S Abbas ◽  
Azza A Moustafa
Keyword(s):  
Capillary Electrophoresis ◽  
Simultaneous Determination ◽  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
British Pharmacopoeia ◽  
Stability Indicating

Abstract Two fast, accurate and selective stability-indicating methods were developed and validated for the simultaneous determination of bisoprolol, perindopril and three of their possible degradation products. The first proposed method was a gradient reversed phase-high-performance liquid chromatography (HPLC) method, whereas the second was a capillary electrophoresis method. The structures of the obtained degradation products were elucidated using infrared and mass spectrometry. They were also confirmed to be either a drug impurity in the British Pharmacopoeia or a precursor to such impurity. The linearity for bisoprolol and perindopril was achieved in the range of 1–20 μg mL−1 and 5–30 μg mL−1 for HPLC and capillary electrophoresis methods, respectively. The proposed methods were validated according to the International Conference on Harmonisation guidelines. The HPLC method proved to be more sensitive and succeeded in the quantitative determination of the obtained degradation products. Also, it was able to quantify perindopril impurity up to three times lower than the desired limit set by the British Pharmacopoeia. They were successfully employed in the determination of bisoprolol and perindopril in their combined pharmaceutical formulation.

scholarly journals A SIMPLE (HPLC–UV) METHOD FOR THE QUANTIFICATION OF COLCHICINE IN BULK AND ETHOSOMAL GEL NANO-FORMULATION AND ITS VALIDATION

2017 ◽  
Vol 9 (7) ◽  
pp. 72 ◽  
Author(s):  
Ibrahim M. Abdulbaqi ◽  
Yusrida Darwis ◽  
Nurzalina Abdul Karim Khan ◽  
Reem Abou Assi ◽  
Gabriel Onn Kit Loh
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Acid Oxidation ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Stress Degradation

Objective: To develop and validate a stability-indicating reversed phase high-performance liquid chromatography (RP-HPLC) method for the determination of colchicine in bulk and ethosomal gel nano-formulation.Methods: The chromatographic conditions were optimized using stainless steel Hypersil Gold C-18 analytical column with the dimensions of 250 mm x 4.6 mm ID x 5 µm. The mobile phase consisted of acetonitrile and ammonium acetate buffer (20 mmol/l, pH=4.85) in the ratio of 32:68 v/v. The flow rate was set at 1 ml/min and the detection wavelength was 353 nm. The column was maintained at 30 °C and the injection volume was 10 µl. The stability of colchicine in different conditions was investigated by exposing the drug to stress degradation using acid, base, oxidation, heat and light.Results: There was no interference from excipients, impurities, dissolution media or degradation products at the retention time of colchicine 5.9 min indicating the specificity of the method. The limit of detection (LOD) and the limit of quantification (LOQ) were 8.64 ng/ml and 26.17 ng/ml respectively. The drug showed good stability under heat, acid, oxidation and light, but substantial degradation was observed under alkali condition. The procedure was validated for specificity, linearity, accuracy and precision.Conclusion: A simple, rapid, specific and stability-indicating HPLC–UV method for the determination of colchicine in the pure and ethosomal gel was successfully developed. The developed method was statistically confirmed to be accurate, precise, and reproducible.

scholarly journals Validation of a liquid chromatographic method for determination of related substances in a candidate certified reference material of captopril

2011 ◽  
Vol 47 (2) ◽  
pp. 351-362 ◽  
Author(s):  
Raquel Nogueira ◽  
Wagner Wollinger ◽  
Thaís Elias da Silva ◽  
Leonardo Mesquita de Oliveira ◽  
Eliane Cristina Pires do Rego ◽  
...  
Keyword(s):  
Reference Material ◽  
Mass Balance ◽  
Certified Reference Material ◽  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Scanning Calorimetry ◽  
Chromatography Method ◽  
Related Substances

This paper describes the validation of a reversed-phase high performance liquid chromatography method (RP-HPLC) with diode array detection (DAD) for determination of related substances (impurities from organic synthesis and degradation products) of captopril according to the Brazilian Pharmacopeia IV. The aim of this study was to guarantee the method accuracy for quantification of related substances, an essential requisite to determine, using the mass balance approach, the captopril content in the first Brazilian certified reference material (CRM) of an active pharmaceutical ingredient (API), developed by Inmetro. The captopril instability in solution is discussed and the captopril content determined by mass balance is compared to the results from titration and differential scanning calorimetry (DSC).

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