Development and validation of a capillary electrophoresis method for the determination of escitalopram and sensitive quantification of its enantiomeric impurity in formulations

Abstract

A rapid capillary zone electrophoresis method has been developed capable of quantifying 0.05% of R-enantiomer and assaying the main component in escitalopram formulations. Many parameters influencing enantioseparation were investigated, which include chiral selectors, buffer composition and pH, applied voltage, capillary length, temperature, and rinsing procedure. Optimal separation conditions were obtained by using a 25 mM phosphate buffer at pH 7.0, containing 1.6% (w/v) sulfated-β-cyclodextrin with short-end injection at 0.5 psi for 5 s. Online UV detection was performed at 205 nm. A voltage of -20 kV was applied and the capillary temperature was kept at 25°C. Separation was achieved in less than 2 min. The method was further validated, including robustness, stability of the solution, selectivity, linearity (escitalopram from 0.25 μg/mL to 600 μg/mL, y = 1528.3 × +1812.9; R² = 0.9999), LOD and LOQ (0.08 and 0.25 μg/mL, respectively), precision and accuracy. The proposed method was then applied to the quality control of the bulk sample and tablets of escitalopram (10 mg).

Development and validation of a high‐performance liquid chromatography–tandem mass spectrometric method for simultaneous determination of bupropion, quetiapine and escitalopram in human plasma

“…Various analytical methods have been reported in the literature to detect each medication separately with their metabolites and/or in combination with other medications in rat and human plasma as well as urine samples. These include gas chromatography (GC; da Fonseca et al ., ), capillary electrophoresis (CE; Deng et al ., ), thin‐layer chromatography (TLC; Soliman and Youssef, ), high‐performance liquid chromatography (HPLC; Belal et al ., ; Yeniceli and Dogrukol‐Ak, ; Suryakant and Sadhana, ), liquid chromatography–mass spectrometry (LC/MS; Zhou et al ., ; Raman et al ., ; Choong et al ., ), gas chromatography–mass spectrometry (GC/MS; Kakde et al ., ), liquid chromatography–tandem mass spectrometry (LC/MS/MS; Moreira et al ., ; Suresh et al ., ; Fisher et al ., ; Pan et al ., ; Parekh et al ., ) and ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC/MS/MS) (Li et al ., ; Tu et al ., ; Denooz et al ., ). However, no method has been reported to simultaneously determine BUP, ESC and QUE in plasma.…”

Capillary electrophoresis in the enantioseparation of modern antidepressants: An overview

“…The method was applied to quality control of bulk sample and tablets of S-CIT, and was capable of quantifying 0.05% of R-CIT (Deng et al, 2012). Analytical parameters influencing chiral separation-CD type and concentration, buffer composition, pH and concentration, applied voltage and temperature-were instigated using the univariate "one factor at time" technique.…”

“…Analytical parameters influencing chiral separation-CD type and concentration, buffer composition, pH and concentration, applied voltage and temperature-were instigated using the univariate "one factor at time" technique. The method was applied to quality control of bulk sample and tablets of S-CIT, and was capable of quantifying 0.05% of R-CIT (Deng et al, 2012).…”

Recent advances in electrodriven enantioseparations

“…Therefore, the quality control of chiral drugs and their products involves also the determination of the unwanted stereoisomer (distomer) in the presence of the active stereoisomer (eutomer). During the reviewed period of time, several reports were published about the application of CE for the determination of enantiomeric purity and/or single active enantiomers in bulk drugs and/or final drug formulations including levocetirizine , ( R )‐modafinil , (–)‐huperzine A , ( R )‐pramipexol , ( R )‐(–)‐chloroquine , RS 86017 , L ‐methotrexate , ( S )‐pantoprazole , and escitalopram . The content of the lipoic acid enantiomers was determined in dietary supplements .…”