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 ◽  
...  

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%.

Author(s):  
Mohamed B. Ali ◽  
Wael Talaat ◽  
Gamal A. Omran ◽  
Hassan A. M. Hendawy ◽  
Samir Morshedy

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.


2014 ◽  
Vol 60 (3) ◽  
pp. 109-115
Author(s):  
Aura Rusu ◽  
G. Hancu ◽  
Á. Gyéresi

Abstract Introduction: Antibacterial quinolones class comprises a series of synthetic antibacterial agents, following the model of nalidixic acid. Because of their common 6-fl uorosubtituent on the quinolone ring, fluroquinolones are the most potent analogues with extended spectrum of activity and great pharmacokinetic properties. The applicability of capillary zone electrophoresis for the separation of fl uoroquinolones in acidic background electrolyte has been studied, our aim being the development of a capillary zone electrophoresis method for the simultaneous separation of six fl uoroquinolones and also to optimize the analytical conditions. The six studied fl uoroquinolones were ciprofloxacin, enoxacin, enrofloxacin, moxifloxacin, ofloxacin and sarafloxacin. Material and methods: Preliminary, we studied the electrophoretic behavior of six fluoroquinolones in an acidic pH, which highlighted the possibility of developing a separation method in this area of pH. Electrophoretic parameters infl uencing separation performance were studied and optimized. Results: A fast and reliable method has been developed, using a background electrolyte containing 100 mM phosphoric acid and the following conditions: applied voltage: + 25 kV, temperature: 20°C, injection pressure 30 mbar - 5 sec, UV detection at 280 nm, capillary: 60 cm (52 cm effective length) x 50 μm, analyte concentration: 167 μg/ml. The separation of the studied fl uoroquinolones was achieved in less than 8 minutes. Conclusions: Capillary zone electrophoresis using an acidic background electrolyte proved to be an efficient tool in the separation of fluoroquinolones from different generations. Also the proposed methods are particular environment-friendly replacement and improvement of a common high performance liquid chromatography determination with rapid analysis time without using any organic solvents.


2014 ◽  
Vol 50 (3) ◽  
pp. 521-527 ◽  
Author(s):  
Brigitta Simon ◽  
Gabriel Hancu ◽  
Árpád Gyéresi

The applicability of capillary electrophoresis for the analysis of four extensively used penicillin derivatives (benzylpenicillin, ampicillin, amoxicillin, oxacilllin) has been studied. Because of structural similarities, the electrophoretic behavior of these derivatives is very similar; consequently an efficient separation using the conventional capillary zone electrophoresis is hard to be achieved. Their simultaneous separation was solved by using micellar electrokinetic capillary chromatography, the separation being based on the differential partition of the analytes between the micellar and aqueous phase. Using a buffer solution containing 25 mM sodium tetraborate and 100 mM sodium dodecyl sulfate as surfactant, at a pH of 9.3, applying a voltage of + 25 kV at a temperature of 25 °C, we achieved the simultaneous separation of the studied penicillin derivatives in less then 5 minutes. The separation conditions were optimized and the analytical performance of the method was evaluated in terms of precision, linearity, limit of detection, and quantification. Also, a simple capillary zone electrophoresis method was applied to study the stability of the studied penicillin derivatives in water at different temperatures, using ciprofloxacin hydrochloride as internal standard. It was observed that the extent of the hydrolysis of penicillins in water is highly dependent on the time and also temperature.


2012 ◽  
Vol 7 ◽  
pp. ACI.S9940 ◽  
Author(s):  
Mohamed Salim ◽  
Nahed El-Enany ◽  
Fathallah Belal ◽  
Mohamed Walash ◽  
Gabor Patonay

A novel, quick, reliable and simple capillary zone electrophoresis CZE method was developed and validated for the simultaneous determination of sitagliptin (SG) and metformin (MF) in pharmaceutical preparations. Separation was carried out in fused silica capillary (50.0 cm total length and 43.0 cm effective length, 49 μm i.d.) by applying a potential of 15 KV (positive polarity) and a running buffer containing 60 mM phosphate buffer at pH 4.0 with UV detection at 203 nm. The samples were injected hydrodynamically for 3 s at 0.5 psi and the temperature of the capillary cartridge was kept at 25 °C. Phenformin was used as internal standard (IS). The method was suitably validated with respect to specificity, linearity, limit of detection and quantitation, accuracy, precision, and robustness. The method showed good linearity in the ranges of 10-100 μg/mL and 50-500 μg/mL with limits of detection of 0.49, 2.11 μm/mL and limits of quantification of 1.48, 6.39 μg/mL for SG and MF, respectively. The proposed method was successfully applied for the analysis of the studied drugs in their synthetic mixtures and co-formulated tablets without interfering peaks due to the excipients present in the pharmaceutical tablets. The method was further extended to the in-vitro determination of the two drugs in spiked human plasma. The estimated amounts of SG/MF were almost identical with the certified values, and their percentage relative standard deviation values (% R.S.D.) were found to be ≤1.50% (n = 3). The results were compared to a reference method reported in the literature and no significant difference was found statistically.


2009 ◽  
Vol 1216 (15) ◽  
pp. 3349-3352 ◽  
Author(s):  
Jennifer P. Pascali ◽  
Eloisa Liotta ◽  
Rossella Gottardo ◽  
Federica Bortolotti ◽  
Franco Tagliaro

2021 ◽  
Vol 2021 ◽  
pp. 1-11
Author(s):  
Thi Thanh Vuong Tong ◽  
Thi Thoa Cao ◽  
Nguyen Ha Tran ◽  
Thi Kim Van Le ◽  
Dinh Chi Le

A green, cost-effective, and simple capillary zone electrophoresis (CZE) method was developed and validated for simultaneous determination of chloramphenicol, methylparaben, and propylparaben in eye-drops. With sodium tetraborate as background electrolyte (BGE), the apparent mobilities of chloramphenicol, methylparaben, and propylparaben increased and analysis time reduced when pH of BGE increased from 8.5 to 10.0 and concentration of BGE decreased from 40 mM to 15 mM, but complete separation of chloramphenicol from other matrix components was achieved only with sodium tetraborate concentration at 30 mM or higher and at pH = 9.3 or lower. The most suitable electrophoretic conditions for the intended application were a 30 mM sodium tetraborate solution, pH 9.3 as BGE, working voltage set at 25 kV, and UV detection at 280 nm at the cathodic extremity of the capillary. The final method was validated and proved to be reliable for assay of chloramphenicol, methylparaben, and propylparaben in eye-drops.


2019 ◽  
Vol 35 (4) ◽  
pp. 55-64
Author(s):  
M.E. Sushkin ◽  
A.S. Simbirtsev

Conditions for analyzing sialylated isoforms of recombinant follicle-stimulating hormone (FSH) by the method of capillary zone electrophoresis have been selected. Follicle-stimulating hormone is a glycosylated heterodimer with the large number of sialic acids that affect its basic biological and physicochemical properties. The optimum protein separation into 6 isoforms was achieved using as a background electrolyte of a solution with pH 4.3 containing 0.01 M trycin, 0.01 sodium chloride, 7 M urea and 2.5 mM 1,4-diaminobutane. follicle-stimulating hormone isoforms, capillary zone electrophoresis, sialic acids, follicle-stimulating hormone.


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