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

2020 ◽  
Vol 32 (4) ◽  
pp. 219-227 ◽  
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.

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

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.

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

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.

scholarly journals Application of Capillary Zone Electrophoresis Coupled with a Diode Array Detector (CZE-DAD) for Simultaneous Analysis of Ibuprofen and Phenylephrine

2019 ◽  
Vol 102 (2) ◽  
pp. 473-479 ◽  
Author(s):  
Marwa A A Ragab ◽  
Mohamed H Abdel-Hay ◽  
Hytham M Ahmed ◽  
Sara M Mohyeldin
Keyword(s):  
Binary Mixture ◽  
Capillary Zone Electrophoresis ◽  
High Efficiency ◽  
Fused Silica ◽  
Simultaneous Analysis ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Zone Electrophoresis ◽  
Capillary Zone

Abstract Background: A validated method based on capillary zone electrophoresis coupled with a diode array detector (CZE-DAD) was investigatedfor analyzing binary mixture of ibuprofen (IBU) andphenylephrine (PHE) in their bulk and combined dosage form. Objective: This binary mixture is a challenging one as IBU is acidic and PHEis alkaline, which may affect their simultaneous analysis using CZE. The literature lacks any CZE report for IBU and PHE simultaneous analysis. Methods: Fused silica capillary (85 cm × 75 μm id) was used, and the electrolyte was a 50 mM borate buffer adjusted to pH 11 with 0.5 M NaOH. Results: The concentration ranges were 5–200 and 5–100 μg/mL for IBU and PHE, respectively, using CZE. High efficiency was achieved (N > 92990). Reasonable migration time (tm) was attained (tm< 8.5 min). Conclusions: Although the results obtained by the proposed CZE method and reported HPLC method were statistically comparable, the proposed method showed lower linearity ranges, higher efficiency, and a more reasonable run time. Highlights: CZE-DAD was used for the analysis of IBU and PHE in bulk and tablets, as no report was foundfor their determination using CZE. Binary mixture is challenging due to differences in chemical and physical properties. A detailed discussion of electrophoretic parameters optimization is included. Confirmation of peak purity was attained using DAD.

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

2019 ◽  
Author(s):  
Wael Talaat ◽  
Hytham Ahmed ◽  
Nahla Salama
Keyword(s):  
Ternary Mixture ◽  
Background Electrolyte ◽  
Pharmaceutical Preparations ◽  
High Sensitivity ◽  
Fused Silica ◽  
Effective Length ◽  
Array Detector ◽  
Internal Diameter ◽  
Pharmaceutical Dosage Forms ◽  
Fused Silica Capillary

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).

scholarly journals Development of a Capillary Electrophoretic Method for the Determination of Huperzine A Concentration in Vietnamese Huperzia serrata

2021 ◽  
Vol 16 (9) ◽  
pp. 1934578X2110332
Author(s):  
Ngoc Chuong Nguyen ◽  
Dinh Vinh ◽  
Duc Tuan Nguyen ◽  
Huynh Van Thi Nguyen ◽  
Cong Luan Tran ◽  
...  
Keyword(s):  
High Efficiency ◽  
Limit Of Detection ◽  
Fused Silica ◽  
Huperzine A ◽  
Effective Length ◽  
Reversible Inhibitor ◽  
Limit Of Quantification ◽  
Electrophoretic Method ◽  
Huperzia Serrata ◽  
Relative Standard

Huperzine A, isolated from Huperzia serrata, is a potent, specific, and reversible inhibitor of acetylcholinesterase with high efficiency and low toxicity. To evaluate the presence of huperzine A in Vietnamese H serrata, a reliable capillary zone electrophoresis method was developed. The analytical conditions were established using 80 mM ammonium acetate buffer, pH 6.0, hydrodynamic injection at 50 mbar for 5 s, applied voltage of 20 kV, temperature at 25 °C, uncoated fused-silica capillary, 56 cm (50 cm effective length) × 70 µm inner diameter, and ultraviolet detection at 310 nm. The recovery rates ranged from 98.05% to 100.64%, with a relative standard deviation <2%. Good linear regression was observed in the concentration range of 1 to 500 µg/mL, with a correlation coefficient of 0.9994. The limit of detection and limit of quantification were 0.33 and 1.0 µg/mL, respectively. These results demonstrate that this method is simple, selective, and suitable for performing quality control for huperzine A derived from Vietnamese H serrata.

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.

scholarly journals High-Throughput Analysis of Lidocaine in Pharmaceutical Formulation by Capillary Zone Electrophoresis Using Multiple Injections in a Single Run

2016 ◽  
Vol 2016 ◽  
pp. 1-6 ◽  
Author(s):  
Andressa C. Valese ◽  
Daniel A. Spudeit ◽  
Maressa D. Dolzan ◽  
Lizandra C. Bretanha ◽  
Luciano Vitali ◽  
...  
Keyword(s):  
Capillary Zone Electrophoresis ◽  
Limit Of Detection ◽  
Background Electrolyte ◽  
Internal Standard ◽  
Effective Length ◽  
Internal Diameter ◽  
Intermediate Precision ◽  
High Throughput Analysis ◽  
Zone Electrophoresis ◽  
Capillary Zone

This paper reports the development of a subminute separation method by capillary zone electrophoresis in an uncoated capillary using multiple injection procedure for the determination of lidocaine in samples of pharmaceutical formulations. The separation was performed in less than a minute leading to doing four injections in a single run. The cathodic electroosmotic flow contributed to reducing the analyses time. The background electrolyte was composed of 20 mmol L−12-amino-2-(hydroxymethyl)-1,3-propanediol and 40 mmol L−12-(N-morpholino)ethanesulfonic acid at pH 6.1. The internal standard used was benzylamine. Separations were performed in a fused uncoated silica capillary (32 cm total length, 23.5 cm effective length, and 50 μm internal diameter) with direct UV detection at 200 nm. Samples and standards were injected hydrodynamically using 40 mbar/3 s interspersed with spacer electrolyte using 40 mbar/7 s. The electrophoretic system was operated under constant voltage of 30 kV with positive polarity on the injection side. The evaluation of some analytical parameters of the method showed good linearity(r2>0.999), a limit of detection 0.92 mg L−1, intermediate precision better than 3.2% (peak area), and recovery in the range of 92–102%.

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

2015 ◽  
Vol 34 (2) ◽  
pp. 267 ◽  
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

<p class="Body"><span lang="EN-US">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 <sup>°</sup>C and the detection was performed at 205 nm wavelenght. Background electrolyte was </span><span lang="EN-US">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 </span><span lang="EN-US">1.0 – 60.0 µg mL<sup>-1</sup> and the limit of detection and quantitation were found as 0.5 and 1.0 µg mL<sup>-1</sup>, respectively. </span></p><p class="Body"><span lang="EN-US"> </span></p>

scholarly journals Validated Method for the Determination of Piroxicam by Capillary Zone Electrophoresis and Its Application to Tablets

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Arın Gül Dal ◽  
Zeynep Oktayer ◽  
Dilek Doğrukol-Ak
Keyword(s):  
Background Electrolyte ◽  
Internal Standard ◽  
Fused Silica ◽  
Electrophoretic Method ◽  
Pharmaceutical Tablets ◽  
Fused Silica Capillary ◽  
Capillary Zone ◽  
The Difference ◽  
Tablet Dosage

Simple and rapid capillary zone electrophoretic method was developed and validated in this study for the determination of piroxicam in tablets. The separation of piroxicam was conducted in a fused-silica capillary by using 10 mM borate buffer (pH 9.0) containing 10% (v/v) methanol as background electrolyte. The optimum conditions determined were 25 kV for separation voltage and 1 s for injection time. Analysis was carried out with UV detection at 204 nm. Naproxen sodium was used as an internal standard. The method was linear over the range of 0.23–28.79 µg/mL. The accuracy and precision were found to be satisfied within the acceptable limits (<2%). The LOD and LOQ were found to be 0.07 and 0.19 µg/mL, respectively. The method described here was applied to tablet dosage forms and the content of a tablet was found in the limits of USP-24 suggestions. To compare the results of capillary electrophoretic method, UV spectrophotometric method was developed and the difference between two methods was found to be insignificant. The capillary zone electrophoretic method developed in this study is rapid, simple, and suitable for routine analysis of piroxicam in pharmaceutical tablets.

scholarly journals Determination of Branched-Chain Amino Acids in Food Supplements and Human Plasma by a CE-MS/MS Method with Enhanced Resolution

2021 ◽  
Vol 22 (15) ◽  
pp. 8261
Author(s):  
Juraj Piestansky ◽  
Michaela Matuskova ◽  
Ivana Cizmarova ◽  
Dominika Olesova ◽  
Peter Mikus
Keyword(s):  
Amino Acids ◽  
Human Plasma ◽  
Limit Of Detection ◽  
Background Electrolyte ◽  
Branched Chain Amino Acids ◽  
Fused Silica ◽  
Suitable Alternative ◽  
Enhanced Resolution ◽  
Validation Parameters ◽  
Branched Chain

In the presented study, a capillary electrophoresis-mass spectrometry method combining high separation efficiency and sensitive detection has been developed and validated, for the first time, to quantify branched chain amino acids (valine, isoleucine, leucine) in commercial food and sport supplement samples and human plasma samples. The separations were performed in a bare fused silica capillary. The background electrolyte was composed of 500 mM formic acid with pH 2.0. The plasma sample pretreatment was realized by simple protein precipitation with acetonitrile. Injection of a short zone of highly basic electrolyte before the sample injection and application of the negative pressure on the separation were accompanied by enhanced resolution of the isobaric amino acids—isoleucine and leucine. The developed method was characterized by favorable validation parameters, such as linearity (r2 > 0.99), accuracy and precision, the limit of detection, lower limit of quantification, or robustness. These parameters were more than sufficient for the quantification of branched chain amino acids in various samples. The determined concentrations of branched chain amino acids in food and sports supplements were in very good agreement with the content declared by the manufacturer. The investigated concentrations of branched chain amino acids were in the range 294.68–359.24 µM for valine, 91.76–95.67 µM for isoleucine, and 196.78–251.24 µM for leucine. These concentrations fall within the physiological limits. The developed CE-MS/MS method represents a suitable alternative to traditional approaches used in branched chain amino acid quality control and bioanalysis.

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