scholarly journals Method Validation for Determination of Metformin Hydrochloride in Pharmaceutical Formulations by Capillary Electrophoresis with Capacitively Coupled Contactless Conductivity Detection

2019 ◽  
pp. 1-10
Author(s):  
Gazala Mohamed Ben-Hander ◽  
Ashraf Ahmed Ali Abdusalam ◽  
Bahruddin Saad ◽  
Ahmad Makahleh ◽  
Salizawati Muhamad Salhimi
Keyword(s):  
Capillary Electrophoresis ◽  
Background Electrolyte ◽  
Pharmaceutical Formulations ◽  
Fused Silica ◽  
Metformin Hydrochloride ◽  
Capacitively Coupled ◽  
Fused Silica Capillary ◽  
Normal Polarity ◽  
C 30

A method for the determination of metformin hydrochloride (MH) in pharmaceutical formulations by capillary electrophoresis with capacitively coupled contactless conductivity (C4D) detection was investigated. The separation was achieved under normal polarity mode at 17.5°C, 30 kV, hydrodynamic injection (50 mbar for 8 s) and using a bare fused silica capillary 72 cm × 75 µm i.d. (detection length, 10.5 cm from the outlet end of the capillary). The optimized background electrolyte consisted of 10 mM 2-morpholinoethanesulfonic acid and 10 mM histidine, pH 6.8. C4D parameters were set at fixed amplitude of 100 V and frequency of 650 kHz. Under the optimum conditions, the method shows good linearity over the range of 10-30 µg mL-1 MH (r2=0.9971). Limits of detection and quantitation based on S/N ratio of 3 and 10 were 0.049 and 0.15 µg mL-1, respectively. The proposed method was successfully applied to the assay of MH in pharmaceutical formulations and establishing the dissolution profiles for both immediate and extended release formulations of MH.

scholarly journals The determination of isoflavones and coumestrol by capillary electrophoresis

2013 ◽  
Vol 19 (No. 4) ◽  
pp. 132-138 ◽  
Author(s):  
J. Moravcová ◽  
T. Kleinová
Keyword(s):  
Capillary Electrophoresis ◽  
Fused Silica ◽  
Biochanin A ◽  
Detector Response ◽  
Two Dimensional ◽  
Nmr Spectrum ◽  
Fused Silica Capillary ◽  
First Time ◽  
Silica Capillary

The separation of six isoflavones (biochanin A, isoformononetin, formononetin, prunetin, daidzein and genistein) and coumestrol on an uncoated fused-silica capillary electrophoresis column was optimised using alkaline borate buffer as electrolyte and DAD detection. A baseline separation of all analytes except a pair, formononetin-biochanin A was achieved at pH 10.5 in 25 min. Detection limits were low (0.1 µg/ml) and the linearity of the detector response was established in the concentration range 0.4–60 µg/ml (180 µg/ml for coumestrol). Coumestrol was synthesized and the carbon signals in 13C-NMR spectrum of both coumestrol and di-O-acetylcoumestrol were assigned for the first time using two-dimensional HMQC technique.

scholarly journals Determination of N-methyl-2-pyrrolidone and its metabolites in urine by micellar electrokinetic chromatography

2011 ◽  
Vol 9 (5) ◽  
pp. 825-833 ◽  
Author(s):  
Jana Lokajová ◽  
Simo Porras ◽  
Eivor Elovaara ◽  
Susanne Wiedmer
Keyword(s):  
Solid Phase ◽  
Background Electrolyte ◽  
Sodium Dodecyl ◽  
Fused Silica ◽  
Rat Urine ◽  
Fused Silica Capillary ◽  
On Line ◽  
Electrokinetic Capillary Chromatography ◽  
Silica Capillary

AbstractA fast and accurate micellar electrokinetic capillary chromatography (MEKC) method was developed for monitoring N-methyl-2-pyrrolidone (NMP) exposure. Baseline separation of NMP and its main metabolites: 5-hydroxy-N-methyl-2-pyrrolidone (5HNMP), N-methylsuccinimide (MSI), 2-hydroxy-N-methylsuccinimide (2HMSI), and 2-pyrrolidone (2P) was obtained within 6 min in an uncoated fused silica capillary using 5 mM phosphate buffer and 140 mM sodium dodecyl sulfate (pH 7.1) as background electrolyte (BGE). On-line UV-detection was performed at 200 nm and the applied electric field was 400 V cm−1. Possible interference of BGE-induced system peaks on separation was investigated by computer simulation and no such interference was observed. The developed MEKC method combined with solid phase extraction for sample preparation was successfully applied to the analysis of urine of rats exposed to NMP. The urinary excretion was determined in 0–6 h and 6–24 h specimens collected after an intragastic administration of 308 mg NMP / kg rat body weight. The results of NMP disposition kinetics in rat urine are reported for NMP and metabolites.

Validated Stability-Indicating Capillary Electrophoresis Method for the Separation and Determination of a Fixed-Dose Combination of Carvedilol and Hydrochlorothiazide in Tablets

2013 ◽  
Vol 96 (5) ◽  
pp. 951-959 ◽  
Author(s):  
Nourah Z Alzoman ◽  
Maha A Sultan ◽  
Hadir M Maher ◽  
Mona M AlShehri ◽  
Ileana V Olah
Keyword(s):  
Capillary Electrophoresis ◽  
Degradation Products ◽  
Background Electrolyte ◽  
Internal Standard ◽  
Fused Silica ◽  
Fixed Dose ◽  
Array Detector ◽  
Forced Degradation ◽  
Stability Indicating

Abstract A novel, fast, sensitive, and specific capillary electrophoresis (CE) technique coupled to a diode array detector has been developed for the separation and simultaneous determination of carvedilol (CRV) and hydrochlorothiazide (HCT) in two combination formulations. The proposed method utilized a fused silica capillary (55 cm × 75 μm id) and the background electrolyte solution phosphate buffer (12.5 mM, pH 7.4)–methanol (95 + 5, v/v). The separation was achieved at 30 kV applied voltage and 24°C. Atorvastatin (80 μg/mL) was chosen as the internal standard. The described method was linear over the range of 1–200 and 0.2–150 μg/mL for CRV and HCT, respectively. Intraday and interday RSD (n = 6) was ≤1.4%. The LOD values of CRV and HCT were 0.26 and 0.07 μg/mL, respectively. The validated CE method was successfully applied to the analysis of two commercial tablet dosage forms. Forced degradation studies were performed on bulk samples of the two drugs using thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. Degradation products produced as a result of stress studies did not interfere with the determination of CRV and HCT; the assay could, therefore, be considered stability-indicating.

Capillary Electrophoresis Method for Determination of Escitalopram Oxalate in Urine Samples and Different Dosage Forms

2020 ◽  
Vol 58 (8) ◽  
pp. 759-769
Author(s):  
Wafa F S Badulla ◽  
Arın G Dal Poçan ◽  
Zeki Atkoşar ◽  
Göksel Arlı
Keyword(s):  
Capillary Electrophoresis ◽  
Limit Of Detection ◽  
Background Electrolyte ◽  
Dosage Forms ◽  
Fused Silica ◽  
Urine Samples ◽  
Effective Length ◽  
Simple Liquid ◽  
Pharmaceutical Dosage Forms

Abstract Application of capillary electrophoresis (CE) has become a rapidly growing analytical technique for the estimation of drugs in pharmaceutical dosage forms and biological fluids. In this study, an effective and sensitive method was developed for the determination of escitalopram oxalate (ESC-OX) by CE with diode-array detection at 200 nm. The separation was achieved by a fused silica capillary with 40 cm effective length (48.5 cm total, 75 μm i.d.). The background electrolyte was composed of 15 mM phosphate buffer (pH 2.5). The applied potential was 22.5 kV, and the samples were injected at 50 mbar pressure for 10 s. Metoprolol was used as an internal standard (IS). The migration time under these optimum conditions was 6.51 ± 0.07 and 6.73 ± 0.08 min for ESC-OX and IS, respectively, with total run time 7 min. The method was validated for linearity, precision, accuracy, specificity and sensitivity. The limit of detection was calculated as 3.85 and 5.07 ng mL−1 for standard and urine samples, respectively. The developed method was employed successfully for the determination of ESC-OX in different pharmaceutical dosage forms and spiked human urine after simple liquid–liquid extraction with good recovery.

Determination of Ferulic Acid in“SHI-QUAN-DA-BU” Pills by High Performance Capillary Electrophoresis

2013 ◽  
Vol 850-851 ◽  
pp. 1152-1155
Author(s):  
Hai Xing Liu ◽  
Qing Liu ◽  
Xiao Yang Xu ◽  
Guo Dong Feng ◽  
Lin Tong Wang ◽  
...  
Keyword(s):  
Capillary Electrophoresis ◽  
Ferulic Acid ◽  
High Performance ◽  
Fused Silica ◽  
Borax Solution ◽  
Fused Silica Capillary ◽  
High Performance Capillary Electrophoresis ◽  
Silica Capillary Column ◽  
Silica Capillary

High performance capillary electrophoresis (HPCE) was used in this text to determine the content of ferulic acid in “SHI-QUAN-DA-BU” Pills. Electrophoretic separation conditions: Uncoated fused silica capillary column(75um×49/58cm), injection height 7.5cm, 30mmol•L-1borax solution, separation voltage 20kV, injection time 15s, detection wavelength 315 nm, experimental temperature 20°C. Linearity was kept in the concentration ranging from 1~31.25 mg·L-1of ferulic acid with correlation coefficient of 0.970. The average recovery was 97.56% and RSD value was 6.4%. The content of ferulic acid was 0.0855 mg/g (n=6).

Fast determination of ethambutol in pharmaceutical formulations using capillary electrophoresis with capacitively coupled contactless conductivity detection

2010 ◽  
Vol 31 (3) ◽  
pp. 570-574 ◽  
Author(s):  
José Alberto Fracassi da Silva ◽  
Nathan Vitorazzi de Castro ◽  
Dosil Pereira de Jesus ◽  
Adriana F. Faria ◽  
Marcus V. N. De Souza ◽  
...  
Keyword(s):  
Capillary Electrophoresis ◽  
Pharmaceutical Formulations ◽  
Conductivity Detection ◽  
Fast Determination ◽  
Capacitively Coupled ◽  
Contactless Conductivity Detection

scholarly journals Development of a Micellar Electrokinetic Chromatographic Method with Indirect UV Detection for Pregabalin Determination in Serum Samples

2018 ◽  
Vol 24 (4) ◽  
pp. 298-303
Author(s):  
Hamid Reza Sargazi ◽  
Elnaz Tamizi ◽  
Elaheh Rahimpour ◽  
Abolghasem Jouyban
Keyword(s):  
Limit Of Detection ◽  
Background Electrolyte ◽  
Fused Silica ◽  
Uv Detection ◽  
Aminosalicylic Acid ◽  
Serum Samples ◽  
Indirect Uv Detection ◽  
Limit Of Quantitation ◽  
Fused Silica Capillary

Background: A micellar electrokinetic chromatographic (MEKC)/ indirect UV detection method with hydrodynamic and electrokinetic injection has been developed for the determination of pregabalin in the serum samples. Methods: Separation of the drug was achieved on Agilent capillary electrophorese in less than 5 min using a 50 cm × 75 μm i.d. uncoated fused-silica capillary and a background electrolyte (BGE) consisting of 5-aminosalicylic acid (5-ASA, 10 mmol L-1), cetyl trimethylammonium bromide (CTAB, 1 mmol L-1) and tri-sodium citrate (4% w/v). The influence of various parameters on the separation such as separation voltage, injection time, cassette temperature, pH of BGE and organic modifier was investigated. Results: Method validation shown good linearity (R2> 0.999) in the range of 1.5-100 µg mL-1 of pregabalin. A limit of detection (LOD) of 0.8 μg mL-1 and a limit of quantitation (LOQ) of 2.6 μg mL-1 were reported for pregabalin. Conclusion: The proposed method was found to be suitable and accurate for the determination of pregabalin in serum samples.

scholarly journals The determination of coumestrol in alfalfa (Medicago sativa) by capillary electrophoresis

2011 ◽  
Vol 48 (No. 5) ◽  
pp. 224-229 ◽  
Author(s):  
J. Moravcová ◽  
T. Kleinová ◽  
R. Loučka
Keyword(s):  
Capillary Electrophoresis ◽  
High Performance ◽  
Solid Phase ◽  
Internal Standard ◽  
Fused Silica ◽  
Detector Response ◽  
Acid Extraction ◽  
Relative Standard ◽  
Fused Silica Capillary

High performance capillary electrophoresis (HPCE) on an uncoated fused-silica capillary column using a&nbsp;borate buffer at pH 9.2 as electrolyte and diode-array detection was developed for the determination of coumestrol in alfalfa. The linear detector response was established in the concentration range 0.76&ndash;140 mg.dm<sup>&ndash;3</sup>, the minimum detectable limit was 0.39 mg.dm<sup>&ndash;3</sup>, and migration time of coumestrol was 5 min. 3-Isobutyl-1-methylxanthin was used as an internal standard. Coumestrol was isolated by acid extraction employing a&nbsp;mixture hydrochloric acid-acetonitrile at 95&deg;C for 30 min followed by solid phase extraction. Relative standard deviations of reproducibility and repeatability were 1.77% and 5.49%, respectively. Spiking recovery value of 92% was achieved. Alfalfa, variety Morava, contains 148&ndash;248 mg.kg<sup>&ndash;1</sup>&nbsp;coumestrol in dry matter. The proposed method is useful for routine analyses.

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