Analysis of ternary mixture of anti-Parkinsonism drugs by capillary electrophoresis in pharmaceutical dosage forms

Abstract A simple CZE method was developed for the analysis of ternary anti-Parkinsonism mixture, levodopa, carbidopa and entacapone. The compounds were simply separated and measured using an untreated fused-silica capillary with 75 μm internal diameter and 85 cm total length, with effective length of 70 cm.. Background electrolyte composed of 20 mM phosphate buffer of pH 7.5 was used under an applied voltage of 15 kV. Photodiode array detector (PDA) was used to identify each compound at different wavelength to obtain high sensitivity. The present method was conducted to the analysis of the ternary mixture in pharmaceutical preparations. The analytical results proved the linearity (r2 ≥ 0.9995), accuracy, precision (% RSD < 2).

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Validated Capillary Zone Electrophoretic Determination of Avanafil and Dapoxetine Hydrochloride in their Pure form and Pharmaceutical Preparation

Journal of Pharmaceutical Research International ◽

10.9734/jpri/2021/v33i46b32960 ◽

2021 ◽

pp. 446-459

Author(s):

Mohamed B. Ali ◽

Wael Talaat ◽

Gamal A. Omran ◽

Hassan A. M. Hendawy ◽

Samir Morshedy

Keyword(s):

Pharmaceutical Preparation ◽

Background Electrolyte ◽

Internal Standard ◽

Fused Silica ◽

Pure Form ◽

Effective Length ◽

Array Detector ◽

Internal Diameter ◽

Capillary Zone ◽

Dapoxetine Hydrochloride

Aims: In this study, a simple, green, and rapid capillary zone electrophoresis (CZE) method coupled with a diode array detector (DAD) was applied for the analysis of avanafil (AVA) and dapoxetine hydrochloride (DAP) as a binary mixture using vardenafil (VAR) as an internal standard (IS) in pure form and pharmaceutical formulation. Methodology: The separation was done using fused silica capillary (58.5 cm total length, 50 cm effective length, and 50 μm internal diameter) and the running background electrolyte (BGE) was 100 mM acetate buffer at pH 3.6. During the separation process, the applied voltage was 30 KV, while the temperature was 25 °C. The sample injection was applied at a pressure of 50 mbar for 10 s, and detection was carried out at 210 nm for DAP and 248 nm for AVA and VAR. Results: Analysis of the tested drugs and the internal standard was carried out in less than 6.5 min, where the migration times were 4.29, 4.90, and 6.02 min for IS, DAP and AVA respectively. The proposed method showed linearity in the concentration range 5-80 and 5-70 μg/mL with correlation coefficients 0.9996 and 0.9999 for AVA and DAP respectively. The limit of detection (LOD) was 0.523 and 0.531 for AVA and DAP respectively, while the limit of quantification (LOQ) was 1.585 and 1.608 in respective order. The Peak purity and identity in the proposed method were validated by DAD. Conclusion: The proposed CZE method was validated according to ICH guidelines and applied successfully for the estimation of AVA and DAP in their combined pharmaceutical preparation.

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Stability-Indicating Micellar Electrokinetic Chromatography Technique for Simultaneous Measurement of Delapril and Manidipine from a Combination Drug Formulation

Journal of AOAC International ◽

10.5740/jaoacint.10-337 ◽

2014 ◽

Vol 97 (1) ◽

pp. 114-120 ◽

Cited By ~ 2

Author(s):

Vítor Todeschini ◽

Maximiliano da Silva Sangoi ◽

Alianise da Silva Meira ◽

Diogo Miron ◽

Alini Dall Cortivo Lange ◽

...

Keyword(s):

Background Electrolyte ◽

Sodium Dodecylsulfate ◽

Internal Standard ◽

Fused Silica ◽

Drug Formulation ◽

Effective Length ◽

Forced Degradation ◽

Combination Drug ◽

Stability Indicating ◽

Fused Silica Capillary

Abstract A stability-indicating micellar electrokineticchromatography (MEKC) method was developed and validated for simultaneous analysis of delapril (DEL) and manidipine (MAN) using salicylic acid as an internal standard. The MEKC method was performed using a fused-silica capillary (effective length of 72 cm) with 50 mM of borate buffer and 5 mM of anionic surfactant sodium dodecylsulfate at pH9.0 as the background electrolyte. The separationwas achieved at 25 kV applied voltage and 35°C. The injection was performed at 50 mbar for5s, with detection at 208 nm. The method was linear in the range of 15–150 μg/mL (r2 = 0.9966) for DEL and 5–50 μg/mL (r2 = 0.9985) for MAN with adequate results for the precision (≤1.87%) and accuracy (98.94% for DEL and 100.65% for MAN). The specificity of the method and its stability-indicating capability was demonstrated through forced degradation studies, which showed that there was no interference from the excipients. The Plackett-Burman experimental design was used for robustness evaluation, giving results within the acceptable range. The method was successfully applied for analysis of the drugs, and the results were compared to an LC method, resulting in nonsignificant differences (P = 0.78 and0.84 for DEL and MAN, respectively).

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Application of MEKC and UPLC with Fluorescence Detection for Simultaneous Determination of Amlodipine Besylate and Bisoprolol Fumarate

Journal of AOAC International ◽

10.1093/jaoacint/qsaa136 ◽

2020 ◽

Author(s):

Sohila M Elonsy ◽

Fawzy A El Yazbi ◽

Rasha A Shaalan ◽

Hytham M Ahmed ◽

Tarek S Belal

Keyword(s):

Simultaneous Determination ◽

Fluorescence Detection ◽

Fused Silica ◽

Effective Length ◽

Fixed Dose ◽

Array Detector ◽

Internal Diameter ◽

Amlodipine Besylate ◽

Validation Parameters

Abstract Objective Two chromatographic methods were described for simultaneous determination of the antihypertensive drugs amlodipine besylate (AML) and bisoprolol fumarate (BIS). Methods Method I applies micellar electrokinetic capillary chromatography using a deactivated fused silica capillary (25 cm effective length × 50 μm internal diameter). The background electrolyte consisted of 0.01 M borate buffer (pH 9.2) containing 0.025 M sodium dodecyl sulphate and methanol in the ratio of 80:20 (v/v). Valsartan (VAL) was used as an internal standard. Diode array detector was set at 238, 224, and 210 nm for measuring AML, BIS, and VAL, respectively. Method II involves using ultra-performance liquid chromatography with fluorescence detection. Zorbax SB-C8 column (2.1 × 100 mm, 1.8 μm particle size) was used with isocratic elution of the mobile phase composed of 0.1% trifluoroacetic acid, acetonitrile, and methanol in the ratio of 55:35:10 (v/v) at a flow rate of 0.6 mL/min. Fluorescence detection was done using excitation wavelengths 230 and 370 nm and emission wavelengths 305 and 450 nm for BIS and AML, respectively. Validation parameters were carefully studied including linearity, ranges, precision, accuracy, robustness, detection, and quantification limits. Results Method I showed good linearity over the range 10–100 μg/mL for both dugs. Method II’s linear ranges were 0.001–0.1 and 0.02–1 µg/mL for BIS and AML, respectively. Conclusion The proposed methods were successfully validated and applied for assay of the studied drugs in their fixed-dose combination tablets. Highlights To the best of our knowledge, this study suggests the first electro-chromatographic and LC with fluorescence detection methods for simultaneous determination of amlodipine and bisoprolol.

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Validated capillary zone electrophoretic method for simultaneous analysis of benazepril in combination with amlodipine besylate and hydrochlorothiazide

Acta Chromatographica ◽

10.1556/1326.2019.00686 ◽

2020 ◽

Vol 32 (4) ◽

pp. 219-227 ◽

Cited By ~ 1

Author(s):

Hytham M. Ahmed ◽

Tarek S. Belal ◽

Rasha A. Shaalan ◽

Fawzy A. El Yazbi ◽

Sohila M. Elonsy

Keyword(s):

Antihypertensive Drugs ◽

Limit Of Detection ◽

Background Electrolyte ◽

Fused Silica ◽

Simultaneous Analysis ◽

Effective Length ◽

Array Detector ◽

Amlodipine Besylate ◽

Electrophoretic Method ◽

Capillary Zone

In this work, a novel, simple, and quick capillary zone electrophoresis (CZE) method was proposed for simultaneous analysis of benazepril (BEN) with other co-administrated antihypertensive drugs, amlodipine besylate (AML) and hydrochlorothiazide (HCT), using a diode array detector (DAD). A fused silica capillary (78.5 cm total length, 70 cm effective length, and 75 μm id) was used in separation using a 40 mM phosphate buffer pH 7.5 as a running background electrolyte (BGE) under a positive potential of 30 KV, at a stable temperature of 25 °C for capillary during separation. Hydrodynamic injections were performed for 12 s at 50 mbar, and detection was performed at 210 nm for AML and BEN, at 225 nm for HCT, and at 232 nm for xipamide (XIP) added as an internal standard (IS). Separation of the three analyzed drugs and the IS was performed in less than 8 min. Migration times were 4.06, 5.23, 6.69, and 7.3 min for AML, HCT, BEN, and XIP, respectively. The findings proved that the proposed method was linear in the range of 10–80 μg/mL for all drugs with correlation coefficients >0.9994. The limit of detection (LOD) values of AML, HCT, and BEN were 1.004, 1.224, and 0.896 μg/mL, respectively, whereas the limit of quantification (LOQ) values were 3.124, 3.727, and 2.749 μg/mL for the cited drugs, respectively. Peak identity and purity were confirmed by DAD. The developed CZE method was applied for the analysis of the three antihypertensive drugs successfully in their combined pharmaceutical tablets, and it can be used for the quality control of single-pill combination (SPC) samples of these drugs in short time.

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

Journal of Chromatographic Science ◽

10.1093/chromsci/bmaa036 ◽

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.

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Evaluation of a capillary electrophoresis method for routine determination of varenicline tartrate in quality control laboratories

Macedonian Journal of Chemistry and Chemical Engineering ◽

10.20450/mjcce.2015.508 ◽

2015 ◽

Vol 34 (2) ◽

pp. 267 ◽

Cited By ~ 2

Author(s):

Mustafa Celebier ◽

Engin Koçak ◽

Sacide Altınöz

Keyword(s):

Limit Of Detection ◽

Background Electrolyte ◽

Internal Standard ◽

Fused Silica ◽

Effective Length ◽

Citrate Buffer ◽

Hydrodynamic Mode ◽

Ich Guidelines ◽

Fused Silica Capillary ◽

Electrophoresis Method

In this study, analyses were carried out in a fused-silica capillary (i.d. 50.0 µm, total length 48.5 cm and effective length 40.0 cm), in normal mode, applying a voltage of 20 kV. Sample injections were made in a hydrodynamic mode over 7 seconds under a pressure of 50 mbar. Capillary temperature was set at 35 °C and the detection was performed at 205 nm wavelenght. Background electrolyte was 40 mM citrate buffer at pH 6.0 and the internal standard was labetalol HCl. Total analysis time was shorter than 5 minutes. The method was validated according to the ICH guidelines and it was found to be linear, precise, accurate, specific, robust and rugged. Linearity range was found to be 1.0 – 60.0 µg mL-1 and the limit of detection and quantitation were found as 0.5 and 1.0 µg mL-1, respectively.

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A Rapid Method for Analysis of Phenylalanine in Cereal Products by MEKC-UV Using LC/MS/MS as a Comparative Method

Journal of AOAC International ◽

10.5740/jaoacint.15-052 ◽

2015 ◽

Vol 98 (6) ◽

pp. 1632-1639 ◽

Cited By ~ 2

Author(s):

Andressa Camargo Valese ◽

Luciano Vitali ◽

Roseane Fett ◽

Gustavo Amadeu Micke ◽

Marcone Augusto Leal de Oliveira ◽

...

Keyword(s):

Comparative Method ◽

Background Electrolyte ◽

Sodium Dodecyl ◽

Fused Silica ◽

Migration Time ◽

Effective Length ◽

Cereal Products ◽

Direct Uv Detection ◽

Fused Silica Capillary ◽

Cereal Samples

Abstract The aim of this study was to develop a new and fast micellar electrokinetic chromatography (MEKC) method for the determination of phenylalanine in cereal samples. The background electrolyte was chosen by a factorial design and was composed of 30 mmol/L phosphoric acid, 100 mmol/L sodium dodecyl sulfate, and 25% methanol (v/v) at pH 1.9. A fused silica capillary (48.5 cm total length × 8.5 cm effective length × 50 μm id × 375 μm od) was used in a short-end injection configuration, and direct UV detection was at 200 nm. The method was validated following the Eurachem guidelines, and values such as linearity (from 10.1 to 40.4 mg/L); recovery (86.8–103.9%); repeatability (0.06–0.22% for migration time and 1.14–4.82% for peak area); reproducibility (0.04–0.61% for migration time and 2.22–5.72% for peak area); and LOD and LOQ of 20 and 60 mg/100 g, respectively, were obtained. After the comparison involving selectivity and accuracy between capillary electrophoresis and LC/MS/MS method, the MEKC-UV method was successfully applied to analysis of phenylalanine in different cereal products.

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Development and Validation of Stability-Indicating GC-FID Method for the Quantitation of Memantine Hydrochloride and Its Nonchromophoric Impurities in Bulk and Pharmaceutical Dosages

Chromatography Research International ◽

10.1155/2012/806068 ◽

2012 ◽

Vol 2012 ◽

pp. 1-10 ◽

Cited By ~ 5

Author(s):

Sanjay A. Jadhav ◽

Shashikant B. Landge ◽

Navanath C. Niphade ◽

Saroj R. Bembalkar ◽

Vijayavitthal T. Mathad

Keyword(s):

Drug Product ◽

High Sensitivity ◽

Bulk Sample ◽

Fused Silica ◽

Stability Indicating ◽

Flame Ionization ◽

Stability Indicating Method ◽

Fused Silica Capillary ◽

The Stability ◽

Development And Validation

A stability-indicating method has been developed and validated for the quantitative determination of memantine hydrochloride and its nonchromophoric impurities in drug substance and drug product using gas chromatography coupled with flame ionization detector (GC-FID). The stability-indicating nature of the method has been proved by establishing peak purity and confirming the mass balance of all samples by subjecting them to stress conditions like hydrolysis, oxidation, photolysis, and thermal degradation studies. The chromatographic separation was performed on a fused silica capillary (HP-5, 30 meter, 0.32 mm and 0.25 μm film thickness) column. The method validation results indicate that the method has acceptable specificity, accuracy, linearity, precision, robustness, and high sensitivity with detection limits and quantitation limits ranging from 0.001% to 0.01% and 0.004% to 0.03%, respectively. The effectiveness of the technique was demonstrated by analysis of different bulk sample of Memantine hydrochloride. The proposed GC-FID method was also found to be specific and selective for the analysis of commercial formulation samples.

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Evaluation of Enantioselective Capillary Electrophoretic Approach for the Enantiomeric Separation of Abscisic Acid

Current Chromatography ◽

10.2174/2213240607999201021123132 ◽

2020 ◽

Vol 7 (1) ◽

pp. 51-56

Author(s):

Atiqah Binti Zaid ◽

Udhayasurya N. Saravanan ◽

Ng Woen Ching ◽

Bahruddin Saad ◽

Yong Foo Wong

Keyword(s):

Abscisic Acid ◽

Higher Plants ◽

Background Electrolyte ◽

Injection Pressure ◽

Enantiomeric Separation ◽

Fused Silica ◽

Electrophoretic Method ◽

Relative Standard ◽

Fused Silica Capillary ◽

Capillary Electrophoretic

Background: The application of enantioselective capillary electrophoresis approach for the assessment of the enantiomeric purity of chiral molecules is receiving increased attention. Abscisic acid is one of the chiral sesquiterpenic plant growth regulators that regulate various ecological and physiological roles in higher plants. Enantiomeric determination of ABA is of great concern because of the different biological activity of its enantiomers. Materials and Methods: In this study, we investigated the enantioseparation selectivity of ABA by incorporating native β-cyclodextrins (β-CD) and its derivatives as chiral modifiers in the background electrolyte of an enantioselective capillary zone electrophoresis system. Electrophoretic aspects that affect the enantiomeric separation, such as pH, types of β-CD and its concentration, applied voltage, injection pressure and time, were studied and optimised. Results and Discussions: An enhancement in enantioseparation was achieved in a bare fused-silica capillary (64.5 cm × 50 mm i.d.) using a background electrolyte solution consisting of (2-hydroxypropyl)- β-CD (80 mM) solubilised in 100 mM phosphate buffer adjusted to pH 5.9 with NaOH, operated under normal polarity mode (25 kV) at 25°C, and using hydrodynamic injection (75 mbar for 10s). Relative standard deviations of (intra- and inter-day) ≤ 3.23% and ≤ 1.39% for migration times and enantiomeric fractions (EF) were achieved using the proposed method. Conclusion: The proposed chiral capillary electrophoretic method offers advantages in terms of enantioselectivity and analysis times, which can serve as a reliable platform for the stereoisomeric analysis of ABA.

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