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

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

10.21203/rs.2.12924/v1 ◽

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).

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

Journal of Analytical Methods in Chemistry ◽

10.1155/2016/4126810 ◽

2016 ◽

Vol 2016 ◽

pp. 1-6 ◽

Cited By ~ 3

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%.

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

Journal of AOAC International ◽

10.5740/jaoacint.11-245 ◽

2013 ◽

Vol 96 (5) ◽

pp. 951-959 ◽

Cited By ~ 4

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.

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

Journal of Analytical Methods in Chemistry ◽

10.1155/2014/352698 ◽

2014 ◽

Vol 2014 ◽

pp. 1-7 ◽

Cited By ~ 6

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.

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Stability-Indicating Methods for Determination of Tiapride in Pure Form, Pharmaceutical Preparation, and Human Plasma

Journal of AOAC International ◽

10.1093/jaoac/90.6.1554 ◽

2007 ◽

Vol 90 (6) ◽

pp. 1554-1565 ◽

Cited By ~ 1

Author(s):

Fadia H Metwally ◽

Mohammad Abdelkawy ◽

Nada S Abdelwahab

Keyword(s):

Human Plasma ◽

Pharmaceutical Preparation ◽

Internal Standard ◽

Reference Method ◽

Pure Form ◽

Stability Indicating ◽

First Derivative ◽

Beer's Law ◽

Beer’S Law

Abstract Four different stability-indicating procedures are described for determination of tiapride in pure form, dosage form, and human plasma. Second derivative (D2), first derivative of ratio spectra (1DD), spectrofluorimetric, and high-performance column liquid chromatographic (LC) methods are proposed for determination of tiapride in presence of its acid-induced degradation products, namely 2-methoxy-5-(methylsulfonyl) benzoic acid and 2-diethylaminoethylamine. These approaches were successfully applied to quantify tiapride using the information included in the absorption, excitation, and emission spectra of the appropriate solutions. In the D2 method, Beer's law was obeyed in the concentration range of 1.59 g/mL with a mean recovery of 99.94 1.38% at 253.4 nm using absolute ethanol as a solvent. In 1DD, which is based on the simultaneous use of the first derivative of ratio spectra and measurement at 245 nm in absolute ethanolic solution, Beer's law was obeyed over a concentration range of 1.59 g/mL with mean recovery 99.64 1.08%. The spectrofluorimetric method is based on the determination of tiapride native fluorescence at 339 nm emission wavelength and 230 nm excitation wavelength using watermethanol (8 + 2, v/v). The calibration curve was linear over the range of 0.23 g/mL with mean recovery of 99.66 1.46%. This method was also applied for determination of tiapride in human plasma. A reversed-phase LC method performed at ambient temperature was validated for determination of tiapride using methanoldeionized watertriethylamine (107 + 93 + 0.16, v/v/v) as the mobile phase. Sulpiride was used as an internal standard at a flow rate of 1 mL/min with ultraviolet detection at 214 nm. A linear relation was obtained over a concentration range of 230 g/mL with mean recovery of 99.66 0.9%. Results were statistically analyzed and compared with those obtained by applying the reference method. They proved both accuracy and precision.

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Simultaneous Separation of 14 Antiarrhythmic Drugs and Determination of Mexiletine and Flecainide by Capillary Zone Electrophoresis

Journal of AOAC International ◽

10.1093/jaoac/90.4.977 ◽

2007 ◽

Vol 90 (4) ◽

pp. 977-986 ◽

Cited By ~ 1

Author(s):

Rafal Pietra ◽

Dorota Kowalczuk ◽

Hanna Hopkala

Keyword(s):

Capillary Zone Electrophoresis ◽

Applied Voltage ◽

Antiarrhythmic Drugs ◽

Fused Silica ◽

Effective Length ◽

Relative Standard ◽

Simultaneous Separation ◽

Zone Electrophoresis ◽

Capillary Zone

Abstract A method using capillary zone electrophoresis was developed for the simultaneous separation of 14 antiarrhythmic drugs belonging to various classes. The drugs are separated on a fused-silica capillary, 90 cm 75 m (72 cm effective length), with phosphate and acetate buffers as background electrolytes and UV detection at 217 nm. The effects of buffer pH, temperature, and applied voltage on the migration of the drugs were studied. The pH was found to be the most significant factor determining effective separation. The antiarrhythmic compounds are completely separated within a relatively short time (<7 min) by using 70 mM phosphate buffer at pH 7.91, an applied voltage of 28 kV, and a temperature of 32C. Mexiletine (MEX) and flecainide (FLE) were quantified under conditions of the optimum separation. The calibration graphs were constructed over the concentration range of 4.014.0 g/mL for both drugs with good correlation (r 0.9999). Detection and quantitation limits were found to be 0.5 and 1.5 g/mL for FLE and 0.7 and 2.1 g/mL for MEX, respectively. The proposed method was used for the determination of both drugs in their commercial forms with satisfactory precision (relative standard deviations of 0.361.21% for FLE and 0.781.66% for MEX) and accuracy (relative standard errors of 0.131.17% for FLE and 0.351.18% for MEX).

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