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

2007 ◽  
Vol 90 (4) ◽  
pp. 977-986 ◽  
Author(s):  
Rafal Pietra ◽  
Dorota Kowalczuk ◽  
Hanna Hopkala

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).

1997 ◽  
Vol 80 (6) ◽  
pp. 1308-1314 ◽  
Author(s):  
Wayne E Rae ◽  
Charles A Lucy

Abstract A capillary zone electrophoresis (CZE) method was developed to separate and determine chlorinated phenols in water and soil samples. A mixture of 16 chlorinated phenols was resolved in 25 min by using a 77 cm (70 cm to detector) × 75 μm fused silica capillary with 0.015M tetraborate/0.045M phosphate (pH 7.3) buffer at 22 kV. Calibration linearities for water samples in the low parts-permillion range were good (correlation coefficient > 0.99) for all solutes except p-chlorophenol. Average precision was 17% relative standard deviation. Typical detection limits were in the 200 μg/L range. Recoveries of chlorinated phenols from synthetic soil samples with methanol were quantitative.


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.


2014 ◽  
Vol 884-885 ◽  
pp. 522-525
Author(s):  
Su Ya Gao ◽  
Li Wang ◽  
Yun Zhang ◽  
Hua Li

A simple and inexpensive high performance capillary zone electrophoresis (CZE) was applied to separate and determine three alkaloids in Radix Aconiti Praeparata simultaneously. The optimized conditions for separation were obtained using 20 mmol/L borax buffer (pH 9.0) containing 2 mmol/L beta-cyclodextrin (β-CD) and 20% methanol. Online UV detection was performed at 235 nm. A voltage of 16 kV was carried at 25°C. Injection was performed at 0.5psi for 10 s. The separation and determination were satisfactory and quick.


2011 ◽  
Vol 361-363 ◽  
pp. 683-686
Author(s):  
Qian Xiang ◽  
Ying Gao

We describe the use of capillary zone electrophoresis (CZE) for the determination of tertiary butylhydroquinone (TBHQ) without derivatization or purification. The influences of buffer pH and voltage on the separation of TBHQ were studied. The internal standard method was used for the quantification of TBHQ. Amperometric detection was carried out at an applied potential of 0.80 V. The detection limit of TBHQ was found to be 10-6 M. Peak intensity varied linearly with TBHQ concentration from 10-4 to 5×10-6 M. The relative standard deviation (RSD) for peak intensity and migration time was in the range of 3.58–4.36% and 0.51–0.94%, respectively. The recovery of the method in food samples is 95.36% for TBHQ. The method developed is suitable for the routine analysis of synthetic phenolic antioxidant TBHQ in samples.


2010 ◽  
Vol 9 (3) ◽  
pp. 410-413
Author(s):  
Adhitasari Suratman ◽  
Hermann Waetzig

The protein separation was studied in capillary zone electrophoresis for preventing protein adsorption on the capillary wall. ß-lactoglobulin (pI: 4.83-5.4, Mr: 18.4 kDa), cytochrome c (pI: 9.59, Mr: 11.7 kDa) and ß-casein (pI: 4.6, Mr: 24 kDa) were used as protein models. Strong adsorption of the proteins occurred onto the capillary at a pH around their pIs. In order to prevent protein adsorption, PEG (Poly(ethylene glycol)) was investigated as an effective substance to stabilize the proteins native state and coat the bare fused-silica capillary surface. The presence of 32 mg/mL PEG in buffer solution in a pH range of 6.0 to 4.0 was successful to suppress protein adsorption during the separation. It can also be confirmed with the reproducibility of apparent EOF mobility with percentile RSD (Relative Standard Deviation) less than 2% in long-term measurement.   Keywords: PEG, protein adsorption, CZE


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