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

2015 ◽  
Vol 98 (6) ◽  
pp. 1632-1639 ◽  
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.

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

2014 ◽  
Vol 97 (1) ◽  
pp. 114-120 ◽  
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).

Simultaneous Determination of Eleven Preservatives in Cosmetics by Micellar Electrokinetic Chromatography

2012 ◽  
Vol 95 (4) ◽  
pp. 1069-1073 ◽  
Author(s):  
Ping Wang ◽  
Xiaojing Ding ◽  
Yun Li ◽  
Uanyuan Ang
Keyword(s):  
Sodium Dodecyl ◽  
Correlation Coefficients ◽  
Sample Pretreatment ◽  
Fused Silica ◽  
New Method ◽  
Effective Length ◽  
Key Factors ◽  
Dehydroacetic Acid ◽  
Fused Silica Capillary ◽  
Electrokinetic Capillary Chromatography

Abstract A new method for the simultaneous quantitation of 11 preservatives—imidazolidinyl urea, benzyl alcohol, dehydroacetic acid, sorbic acid, phenoxyethanol, benzoic acid, salicylic acid, and four parabens (methyl, ethyl, propyl, and butyl)—in cosmetics by micellar electrokinetic capillary chromatography was established and validated. The separation was performed using an uncoated fused-silica capillary (50 μm id × 60.2 cm, effective length 50 cm) with a running buffer consisting of 15 mmol/L sodium tetraborate, 60 mmol/L boric acid, and 100 mmol/L sodium dodecyl sulfate. A 1:10 dilution of the running buffer was used as the sample buffer to extract the cosmetic samples. The key factors, such as the concentration and pH of the running and sample buffers, which influence quantitative analysis of the above 11 preservatives in cosmetic samples, were investigated in detail. The linear ranges of the calibration curves for imidazolidinyl urea and the other 10 preservatives were 50–1000 and 10–200 mg/L, respectively. The correlation coefficients of the standard curves were all higher than 0.999. The recoveries at the concentrations studied ranged from 93.0 to 102.7%. RSDs were all less than 5%. The new method with simple sample pretreatment met the needs for routine analysis of the 11 preservatives in cosmetics.

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.

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 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 Development of alternative methods for the determination of raloxifene hydrochloride in tablet dosage form

2015 ◽  
Vol 51 (2) ◽  
pp. 349-360 ◽  
Author(s):  
Fernanda Rodrigues Salazar ◽  
Cristiane Franco Codevilla ◽  
Leonardo Meneghini ◽  
Ana Maria Bergold
Keyword(s):  
Dosage Form ◽  
Background Electrolyte ◽  
Sodium Dodecyl ◽  
Fused Silica ◽  
Uv Detection ◽  
Effective Length ◽  
Alternative Methods ◽  
Pharmaceutical Dosage Form ◽  
Raloxifene Hydrochloride

<p>Three methods are proposed for the quantitative determination of raloxifene hydrochloride in pharmaceutical dosage form: ultraviolet method (UV) high performance liquid chromatography (HPLC) and micellar capillary electrophoresis (MEKC). These methods were developed and validated and showed good linearity, precision and accuracy. Also they demonstrated to be specific and robust. The HPLC and MEKC methods were tested in regards to be stability indicating methods and they showed to have this attribute. The UV method used methanol as solvent and optimal wavelength at 284 nm, obeying Lambert-Beer law in these conditions. The chromatographic conditions for the HPLC method included: NST column C18 (250 x 4.6 mm x 5 µm), mobile phase water:acetonitrile:triethylamine (67:33:0,3 v/v), pH 3.5, flow rate 1.0 mL min<sup>-1</sup>, injection volume 20.0 µl, UV detection 287 nm and analysis temperature 30 °C. The MEKC method was performed on a fused-silica capillary (40 cm effective length x 50 µm i.d.) using as background electrolyte 35.0 mmol L<sup>-1</sup> borate buffer and 50.0 mmol L<sup>-1</sup> anionic detergent sodium dodecyl sulfate (SDS) at pH 8.8. The capillary temperature was 32°C, applied voltage 25 kV, UV detection at 280 nm and injection was perfomed at 45 mBar for 4 s, hydrodimanic mode. In this MEKC method, potassium diclofenac (200.0 µg mL<sup>-1)</sup> was used as internal standard. All these methods were statistically analyzed and demonstrated to be equivalent for quantitative analysis of RLX in tablets and were successfully applied for the determination of the drug.</p>

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.

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

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.

scholarly journals Comparison of Three Analytical Methods for Quality Control of Clozapine Tablets

2001 ◽  
Vol 84 (2) ◽  
pp. 361-367 ◽  
Author(s):  
Maria Augusta Raggi ◽  
Vincenzo Pucci ◽  
Francesca Bugamelli ◽  
Vittorio Volterra
Keyword(s):  
Quality Control ◽  
Analytical Methods ◽  
Phosphate Buffer ◽  
Supporting Electrolyte ◽  
Background Electrolyte ◽  
Reversed Phase ◽  
Fused Silica ◽  
Intermediate Precision ◽  
Fused Silica Capillary ◽  
Liquid Chromatographic

Abstract Three different analytical methods for the quality control of clozapine in commercial formulations were developed and compared: a liquid chromatographic (LC) method with UV detection, a capillary zone electrophoretic (CZE) method, and a linear scan voltammetric (LSV) method. The isocratic LC procedure used a C18 reversed-phase column; the CZE method used an uncoated fused-silica capillary and phosphate buffer containing polyvinylpyrrolidone as the background electrolyte; the LSV method analyzed clozapine solutions with acidic phosphate buffer as the supporting electrolyte. The 3 methods gave similar and satisfactory results, in terms of precision and accuracy. Repeatability and intermediate precision were good (RSD% &lt; 2.2) and accuracy, resulting from recovery studies, was between 98 and 102%. The rapidity of analysis was high for all 3 methods, especially for the LSV.

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