scholarly journals Determination of enantiomeric purity of esomeprazole by capillary electrophoresis

2020 ◽  
Vol 93 (2) ◽  
pp. 93-101
Author(s):  
Papp Lajos Attila ◽  
Hancu Gabriel ◽  
Kelemen Hajnal ◽  
Gyéresi Árpád
Keyword(s):  
Capillary Electrophoresis ◽  
Proton Pump ◽  
Chiral Separation ◽  
Benzimidazole Derivative ◽  
Pharmaceutical Preparations ◽  
Cost Effective ◽  
Enantiomeric Purity ◽  
Separation Method ◽  
Electrophoretic Behavior

Abstract Proton pump inhibitors are the most effective agents used in gastric hyper-acidity-related disorders. Omeprazole is a benzimidazole-derivative compound with an asymmetric sulphur in its structure, which generates its chiral character. Esomeprazole (S-omeprazole) was the first proton pump inhibitor introduced as an enantiomerically pure compound in therapy, after the successful chiral switch of the racemic omeprazole. This work is aimed at performing a complementary study to an already published chiral separation method of omeprazole. As preliminary analysis, the electrophoretic behavior of omeprazole enantiomers and the possible mechanism of the chiral resolution was studied using different background electrolytes containing different β-cyclodextrin derivatives, as chiral selectors. The robustness of the chiral separation method was tested by applying a Plackett-Burman design. The method was validated according to current ICH guidelines and proved to be reliable, linear, precise and accurate for the determination of 0.2% R-omeprazole as chiral impurity in esomeprazole samples. The validated method was successfully used for the analysis of esomeprazole-containing gastro-resistant tablets. According to our results, valuable information on the mechanism of chiral separation of omeprazole was gained and the application area of the previously developed method was successfully enlarged. The presented rapid and cost-effective capillary electrophoresis method proved to be suitable for the determination of enantiomeric purity of esomeprazole from pharmaceutical preparations and could represent an alternative for the available compendial methods.

scholarly journals Cost-Effective Potentiometric Platforms Modified with Multi-Walled Carbon Nanotubes (MWCNTs) and Based on Imprinted Receptors for Fluvoxamine Assessment

Polymers ◽  
2020 ◽  
Vol 12 (3) ◽  
pp. 673
Author(s):  
Heba M. Hashem ◽  
Saad S. M. Hassan ◽  
Ayman H. Kamel ◽  
Abd El-Galil E. Amr ◽  
E. M. AbdelBary
Keyword(s):  
Carbon Nanotubes ◽  
Electrochemical Impedance ◽  
Biological Fluids ◽  
Pharmaceutical Preparations ◽  
Cost Effective ◽  
Hplc Method ◽  
Multi Walled Carbon Nanotubes ◽  
Walled Carbon Nanotubes ◽  
Screen Printed

A simple, efficient and reliable analytical method was developed and used for the determination of the fluvoxamine drug (FLV) in pharmaceutical preparations and biological fluids. The method is based on the cost-effective screen-printed platform for the potential transduction of the drug. Host-tailored molecular imprinting polymer (MIP) was integrated with the potentiometric platform as a recognition receptor, in which FLV, acrylamide (AAm), ethylene glycol dimethacrylate (EGDMA) and acetonitrile were used as a template, functional monomer, cross-linker, and solvent, respectively. MIP particles were dispersed in plasticized poly (vinyl chloride) (PVC) and the membrane was drop-casted on carbon screen-printed electrode. The MIP, in addition to non-imprinted polymers (NIP), was characterized and the binding experiment revealed high affinity and adsorption capacity of MIP towards FLV. The proposed sensor displayed near-Nernstian cationic slope of 55.0 ± 0.8 mV/decade (r2 = 0.999) with a low detection limit of 4.8 × 10−6 mol/L over a wide pH range (3.0–8.5). The electrochemical features of the proposed sensors including electrochemical impedance spectroscopy (EIS) and chronopotentiometry measurements (CP) in the presence of multi-walled carbon nanotubes (MWCNTs) as a solid contact transducer were also investigated. The applications of the proposed sensor for the determination of FLV in different dosage forms with recovery values (98.8%–101.9%) and (97.4%–101.1%), respectively compared with the reference HPLC method with acceptedFandt-student tests values at the 95% confidence level.

scholarly journals Development and Validation of a Chiral HPLC Method for Quantitative Analysis of Enantiomeric Escitalopram

2018 ◽  
Vol 16 (2) ◽  
pp. 165-172 ◽  
Author(s):  
Asma Rahman ◽  
Mohammad Rashedul Haque ◽  
M Muhibur Rahman ◽  
Mohammad A Rashid
Keyword(s):  
Pharmaceutical Preparations ◽  
Enantiomeric Separation ◽  
Hplc Method ◽  
Enantiomeric Purity ◽  
Chiral Hplc ◽  
Average Percentage ◽  
Quantitation Limit ◽  
Relative Standard ◽  
Development And Validation

In the present study a rapid, accurate and precise chiral HPLC method was developed and validated for enantiomeric separation of racemate citalopram and escitalopram according to the guidelines of United States of Pharmacopeia (USP) and International Conference on Harmonization (ICH). The chiral chromatographic separation was achieved with ammonium acetate/ ethanol/ 2-propanol/ methylene dichloride (100 : 150 : 70 : 30, v/v) at a flow rate of 0.5 ml/min using a chiral CD-PH column. The HPLC analyses were monitored at 254 nm. The method showed a good linearity with regression coefficient (r2) of 0.998 in the range of 20.0-70.0 μg/ml for escitalopram. The detection limit (LOD), quantitation limit (LOQ) and average percentage of recovery for escitalopram were found to be 2.54, 7.68 μg/ml and 100.28% to 102.86%, respectively. The percentage of relative standard deviation (%RSD) for intra- and inter- day precision were found as 0.16% and 0.09%, respectively. The established method proved as reproducible with a %RSD value of less than 2 and having the robustness within specified limit. The present study also showed the enantiomeric purity or excess (%ee) of seven pharmaceutical preparations of escitalopram. Thus the proposed chiral method can be applied for the enantiomeric purity determination of escitalopram formulations.Dhaka Univ. J. Pharm. Sci. 16(2): 165-172, 2017 (December)

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