scholarly journals Development of a Capillary Electrophoresis Method for the Enantioselective Estimation of Primaquine in Pharmaceutical Formulations

2008 ◽  
Vol 91 (3) ◽  
pp. 536-541 ◽  
Author(s):  
Abdalla A Elbashir ◽  
Bahruddin Saad ◽  
Abdussalam Salhin Mohamed Ali ◽  
Muhammad Idiris Saleh
Keyword(s):  
Capillary Electrophoresis ◽  
Applied Voltage ◽  
Pharmaceutical Formulations ◽  
Fused Silica ◽  
Chiral Selector ◽  
Effective Length ◽  
Racemic Mixture ◽  
Injection Time ◽  
Relative Standard ◽  
Capillary Temperature

Abstract A capillary electrophoresis (CE) method has been developed that allows the separation and estimation of primaquine enantiomers using hydroxypropyl--cyclodextrin (HP--CD) as a chiral selector. The influence of chemical and instrumental parameters on the separation, such as type and concentration of CD, buffer concentration, buffer pH, applied voltage, capillary temperature, and injection time, were investigated. Good separation of the racemic mixture of primaquine was achieved using a fused-silica capillary (52.5 cm effective length 50 m id) and a background electrolyte composed of tris-phosphate buffer solution (50 mM, pH 2.5) containing 15 mM HP--CD as a chiral selector. The recommended applied voltage, capillary temperature, and injection time were 15 kV, 25C, and 6 s, respectively. Within-day and interday reproducibility of peak area and migration time gave relative standard deviation values ranging from 1.053.30. Good recoveries (range of 96.8104.9) were obtained from the determination of placebos that were spiked with 0.251.00 mg/L primaquine. The proposed CE method was successfully applied to the assay of primaquine diphosphate in pharmaceutical formulations (tablets).

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
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).

Capillary electrophoresis of wheat gliadin proteins and its potential for wheat varietal identification using pattern matching software

2001 ◽  
Vol 52 (8) ◽  
pp. 839 ◽  
Author(s):  
S. Siriamornpun ◽  
M. Wootton ◽  
J. M. Cox ◽  
F. Bekes ◽  
C. W. Wrigley
Keyword(s):  
Capillary Electrophoresis ◽  
Pattern Matching ◽  
Processing Parameters ◽  
Peak Height ◽  
Fused Silica ◽  
Constant Current ◽  
Good Resolution ◽  
Relative Mobility ◽  
Window Width ◽  
Relative Standard

Gliadins from 11 wheat flours were extracted with 30% ethanol and fractionated by capillary electrophoresis on a 20-µm i.d. untreated fused silica capillary using 0.1 M phosphate buffer (pH 2.5) containing polymer modifier. Capillary electrophoresis conducted at a constant current provided very good resolution and reproducibility (relative standard deviation <0.5) in mp;lt;15 min. Pattern matching of the profiles was performed with the PatMatch program to provide quantitative comparisons, using the relative mobility and intensity data for each gliadin protein. Data processing parameters, including the integration of the electrophoregram, were optimised for separation of gliadins extracted from either whole-grain or flour samples. The reproducibility and repeatability were compared using peak height and/or area percentages. The optimal window width for identifying matching gliadin peaks was 0.80–1.20% relative mobility units. Using these conditions, it was concluded that unknown varieties could be identified with a confidence level of 90–95%.

scholarly journals Using a surface response method for experimental design to optimize the analysis of taurine in food supplements by capillary electrophoresis

2017 ◽  
Vol 33 (4) ◽  
Author(s):  
Nguyen Manh Huy ◽  
Nguyen Thanh Dam ◽  
Duong Hong Anh ◽  
Pham Hung Viet
Keyword(s):  
Capillary Electrophoresis ◽  
Ph Value ◽  
Milk Powder ◽  
Energy Drink ◽  
Injection Time ◽  
Sample Injection ◽  
Surface Response ◽  
Relative Standard ◽  
Surface Response Method ◽  
Response Method

Abstract: This study focus on using surface response method to optimize the taurine analysis by capillary electrophoresis with contactless conductivity detector. A response surface method (RSM) coupled with a central composite model (CCD) comprising 30 experiments was developed with 4 factors including concentration of Tris buffer, pH value, separating potential and sample injection time. The best set of factor levels for taurine analysis was found as follows: 150 mmol/L of Tris concentration, pH = 8.96, separation voltage of -10 kV, the sample injection time of 60 seconds. The validation of analytical method showed the detection limit for taurine was 0.266mg/L, linearity range from 1 to 500 mg/L, relative standard deviation values ​​for peak areas and migration times were less than 3.16%, the linear correlation coefficient gained 0.999. Recovery efficiency of taurine in several food supplement matrixes such as: fresh milk, milk powder, energy drink were in range from 91.9% to 101.7%.  

Capillary Electrophoresis Methods for the Determination of Tramadol: A Review

2019 ◽  
Vol 25 (4) ◽  
pp. 278-286
Author(s):  
Anita Sarkany ◽  
Gabriel Hancu ◽  
Claudiu Drăguț ◽  
Adriana Modroiu ◽  
Enikő Barabás-Hajdu
Keyword(s):  
Capillary Electrophoresis ◽  
Opioid Analgesic ◽  
Cost Effective ◽  
Pharmaceutical Formulations ◽  
Racemic Mixture ◽  
Effective Solution ◽  
Complex Mechanism ◽  
Biological Matrices ◽  
Opiate Agonist

Tramadol is a widely used opioid analgesic frequently prescribed for treatment of moderate to severe, acute and chronic pain. It has a complex mechanism of action, acting both as a central opiate agonist and as a norepinephrine and serotonin reuptake inhibitor. It is a chiral substance, having two chiral centers in its structure and it is used in therapy as a racemic mixture of two of its enantiomers, (S,S)-tramadol and (R,R)-tramadol. In the last 25 years, several analytical procedures have been published in the literature for the achiral and chiral determination of tramadol from pharmaceutical formulations and biological matrices. Among these methods, capillary electrophoresis techniques have proved to be an efficient, reliable and cost-effective solution. The purpose of the present review is to provide a systematic survey to present and discuss the electrodriven methods available in the literature for the achiral and chiral analysis of tramadol.

scholarly journals The Use of Single Drop Microextraction and Field Amplified Sample Injection for CZE Determination of Homocysteine Thiolactone in Urine

Molecules ◽  
2021 ◽  
Vol 26 (18) ◽  
pp. 5687
Author(s):  
Krystian Purgat ◽  
Izabella Kośka ◽  
Paweł Kubalczyk
Keyword(s):  
Calibration Curve ◽  
Phosphate Buffer ◽  
Fused Silica ◽  
Effective Length ◽  
Single Drop ◽  
Homocysteine Thiolactone ◽  
Sample Injection ◽  
Single Drop Microextraction ◽  
Relative Standard

Two cheap, simple and reproducible methods for the electrophoretic determination of homocysteine thiolactone (HTL) in human urine have been developed and validated. The first method utilizes off-line single drop microextraction (SDME), whereas the second one uses off-line SDME in combination with field amplified sample injection (FASI). The off-line SDME protocol consists of the following steps: urine dilution with 0.2 mol/L, pH 8.2 phosphate buffer (1:2, v/v), chloroform addition, drop formation and extraction of HTL. The pre-concentration of HTL inside a separation capillary was performed by FASI. For sample separation, the 0.1 mol/L pH 4.75 phosphate buffer served as the background electrolyte, and HTL was detected at 240 nm. A standard fused-silica capillary (effective length 55.5 cm, 75 μm id) and a separation voltage of 21 kV (~99 μA) were used. Electrophoretic separation was completed within 7 min, whereas the LOD and LOQ for HTL were 0.04 and 0.1 μmol/L urine, respectively. The calibration curve in urine was linear in the range of 0.1–0.5 μmol/L, with R2 = 0.9991. The relative standard deviation of the points of the calibration curve varied from 2.4% to 14.9%. The intra- and inter-day precision and recovery were 6.4–10.2% (average 6.0% and 6.7%) and 94.9–102.7% (average 99.7% and 99.5%), respectively. The analytical procedure was successfully applied to the analysis of spiked urine samples obtained from apparently healthy volunteers.

A Friendly Environmental CE Method to Determine Doxycycline Hyclate in Suppositories and Application to Tablet Assay

2019 ◽  
Vol 15 (5) ◽  
pp. 531-539 ◽  
Author(s):  
Ana P. Christ ◽  
Sulen L. Burin ◽  
Andréa I.H. Adams
Keyword(s):  
Degradation Products ◽  
Fused Silica ◽  
Effective Length ◽  
Official Method ◽  
Good Resolution ◽  
Doxycycline Hyclate ◽  
Related Substance ◽  
Relative Standard ◽  
Fused Silica Capillary ◽  
Electrophoresis Method

Background: The demand for green analytical methods is rising, mainly due its impact on the reduction of waste generation. The official method to assay Doxycycline Hiclate (DOXH) is HPLC, using an unusual column and a multi-component mobile phase. Objective: To develop a capillary electrophoresis method (CZE) to assay DOXH in suppositories and tablets. Methods: Doxycycline was analyzed in a CZE system using a fused silica capillary silica (effective length 40 cm), voltage 25kV, temperature 24°C, detection at 260 nm and hydrodynamic injection of 50mBar/5s. The electrolyte was a mixture of acetonitrile and aqueous solution composed of 25 mM sodium carbonate and 5mM EDTA, pH 10.6. Results: The method was validated according to ICH requirements and DOXH detection was achieved at around 5 min. A linear relationship was observed in the range of 20 to 160 µg.mL-1, the method was precise, showing values of relative standard deviation below 2%. Accuracy was demonstrated by DOXH recovery values ranging from 98.0 to 102.0%, for all the formulations. The specificity was studied by the peak purity evaluation and by the good resolution between peaks of DOXH, degradation products and a related substance intentionally added to the sample solution. Robustness was evaluated by 23 full factorial design, and no effect on DOXH assay was observed under simultaneous variation in significant analytical parameters. Conclusion: This simple and inexpensive method may be used to determine DOXH in suppositories as well tablets, under identical analytical conditions and can be a green alternative to the HPLC official method.

Chiral Separation of Non-Natural Amide Amino Acid by Capillary Electrophoresis with CD Derivations as Chiral Selective Material

2012 ◽  
Vol 554-556 ◽  
pp. 824-827 ◽  
Author(s):  
Bao Hui Li
Keyword(s):  
Capillary Electrophoresis ◽  
Amino Acid ◽  
Chiral Separation ◽  
Fused Silica ◽  
Effective Length ◽  
Separation Of Enantiomers ◽  
Chiral Selectivity ◽  
Fused Silica Capillary ◽  
Silica Capillary

A capillary electrophoresis (CE) method for the separation of four kinds of enantiomers of non-natural carboxylic amino acid was built while hydroxypropyl-β- cyclodextrin (HP-β-CD) derivations as chiral selective material. Several different β-CD derivatives were tested for the chiral separation of non-natural carboxylic amino acid, and it was proved that HP-β-CD could show better chiral selectivity. The separation of enantiomers of amino acid was obtained by CE in a 50-μm i.d.×60 cm (effective length 45 cm) fused-silica capillary at 18 kV voltage, while 10 mM phosphate acted as running buffer and HP-β-CD served as selective material. The detective wavelength was set at 254 nm.

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.

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