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  • Author: Anca Gabriela Cârje x
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Open access

Alina Balint, Anca Gabriela Cârje, Daniela Lucia Muntean and Silvia Imre

Abstract

Objective: The aim of the study was to compare the influence of mobile phase composition and temperature on chiral separation of racemic ibuprofen by capillary electrophoresis and high performance liquid chromatography with UV detection. Materials and methods: Racemic ibuprofen was analysed on a chiral OVM column with an HPLC system 1100 Agilent Technologies, under isocratic elution, by using potassium dihydrogen phosphate 20 mM and ethanol in mobile phase. The flow rate was set at 1 mL/min, UV detector at 220 nm and different column temperatures were tested. For electrophoresis separation an Agilent CE G1600AX Capillary Electrophoresis System system, with UV detection, was used. The electrophoresis analysis was performed at different pH values and temperatures, with phosphate buffer 25 mM and methyl-β-cyclodextrin as chiral selector. Results: The chromatograhic analysis reveals a high influence of mobile phase pH on ibuprofen enantiomers separation. An elution with a mixture of potassium dihydrogen phosphate 20 mM pH=3 and ethanol, at 25°C, allowed enantiomers separation with good resolution in less than 8 min. Conclusions: The proposed HPLC method proved suitable for the separation of ibuprofen enantiomers with a good resolution, but the capillary electrophoresis tested parameters did not allow chiral discrimination.

Open access

Paula Antonoaea, Anca Gabriela Cârje, Adriana Ciurba, Nicoleta Todoran, Alexandru Robert Vlad and Daniela Lucia Muntean

Abstract

Objective: The aim of this study was to develop and validate two HPLC methods for the quantification of meloxicam and tenoxicam from transdermal therapeutic systems.

Methods: Based on 1.0% hydroxypropyl methylcellulose 15000, transdermal patches containing meloxicam or tenoxicam were prepared by solvent evaporation technique. Analytical performances of the HPLC methods for the quantification of meloxicam and tenoxicam from such systems were assessed in terms of specificity, linearity, detection limit, quantification limit, recovery and precision.

Results and discussion: The linearity of the method was assessed through a calibration curve in the 1.0 - 75.0 μg∙mL−1 concentration range, with a regression coefficient higher than 0.999. The detection limit and the quantification limit were found to be 0.46 μg∙mL−1 and 1.39 μg∙mL−1, for meloxicam; and 0.88 μg∙mL−1, respectively 2.64 μg∙mL−1 for tenoxicam. According to the European Pharmacopeia 5.0 the mean recovery was found to be between 75% and 125%. As performance criteria for precision was used the RSD% which were lower than 2.0% for both methods.

Conclusions: The proposed liquid chromatography methods provide selective, linear and precise results for the quantification of meloxicam and tenoxicam from transdermal therapeutic systems. The presence of a single peak in the chromatograms of the analyzed transdermal patches with meloxicam or tenoxicam, certify the successful determination of the active pharmaceutical ingredient in the prepared patches.

Open access

Ion Valentin, Imre Silvia, Cârje Anca Gabriela and Muntean Daniela Lucia

Abstract

Introduction: Perindopril, as an angiotensin converting enzyme inhibitor and indapamide, as a thiazide like diuretic, can be administrated together for the treatment of high blood preasure and other cardiovascular diseases. The aim of this study was to develop two simple and reliable separation methods for perindopril and indapamide by high performance liquid chromatography and capillary zone electrophoresis in order to evaluate their behaviour under separation conditions, for simultaneous separation.

Materials and methods: Standard solutions of perindopril erbumine and indapamide in proper solvents were analized. An Agilent 1100 series HPLC system was used for the separation of the two analytes on a C18 stationary phase (Zorbax Stable Bond 3.5 µm), under an isocratic elution. As a comparative method, an Agilent 7100 series capillary electrophoresis system was used for the development of the electrophoretic method.

Results: Both developed methods turned to comply to the separation performance parameters such as resolution and selectivity, with low limits of detection, wide range of liniarity. No statistical difference concerning precision of the qualitative parameters was observed. Time analysis less than 5 minutes both for chromatographic and electrophoretic separations proved to generate cost and time effective analysis methods.

Conclusions: Two analytical methods, HPLC and CZE respectively, for the separation of perindoprile erbumine and indapamide have been successfully developed, both recording satisfactory analytical parameters.

Open access

Anca Gabriela Cârje, Alina Balint, Daniela-Lucia Muntean, Gabriel Hancu, Valentin Ion and Silvia Imre

Abstract

Objective: The purpose of this study was to separate the enantiomers of amlodipine by High Performance Liquid Chromatography (HPLC) using ovomucoid (OVM) as chiral selector, respectively by Capillary Electrophoresis (CE) using cyclodextrines and to evaluate the analytical performance of the both proposed methods.

Material and methods: HPLC enantioseparation of amlodipine was performed on an HPLC Agilent Technologies 1100 series using as chiral stationary phase an Ultron ES OVM, 150x4.6 mm column with ovomucoid as chiral selector. The stereoselective CE analysis of amlodipine was achieved on Agilent Technologies 7100 CE using uncoated fused-silica capillaries 48 cm x 50 mm and different type of cyclodextrins as chiral selectors.

Results: A mobile phase consisting of 80% Na2HPO4 10 mM at a pH level of 5.0 and 20% ACN, isocratic elution at a flow of 1 ml/min turned to be the optimal experimental conditions for HPLC analysis (R=5.51; α=1.71) with retention times shorter than 10 minutes for the two isomers, tR (S-AML) = 4.63 (min); tR (R-AML) = 5.54 (min). The migration times for amlodipine enantiomers were tm (S-AML) = 8.15 (min) and tm (R-AML)= 8.45 (min) and the optimum CE conditions have proven to be a buffer solution containing 25 mM H3PO4 at pH 3.0 and 20 mM α-CD as chiral selector and a capillary temperature set at 15°C (R=1.51; α=1.03).

Conclusion: The analytical performances of the chromatographic method using OVM as chiral selector are superior to the electrophoretic analysis method but the CE method is more economical and may represent an alternative to the HPLC chromatographic separation.