New validated HPLC methodology for the determination of (−)-trans-paroxetine and its enantiomer in pharmaceutical formulations with use of ovomucoid chiral stationary phase

Abstract

A new chromatographic method for the enantioseparation and the determination of (−)-trans-paroxetine and (+)-trans-paroxetine has been developed with the aid of amylose ovomucoid-based chiral stationary phase. The method is faster and five times more sensitive than procedures recommended previously: limit of detection and limit of quantification are 5 and 16 ng/mL, respectively [modified (Ferretti et al. in J Chromatogr B 710:157–164, 1998): 20 and 60 ng/mL]. It was carefully validated and applied for the determination of (−)-trans-paroxetine and (+)-trans-paroxetine in Parogen (Mc Dermott Laboratories Ltd.) and Xetanor (Actavis) coated tablets.FigureᅟElectronic supplementary materialThe online version of this article (doi:10.1007/s00216-013-7565-y) contains supplementary material, which is available to authorized users.

EnantioselectiveLCanalysis and determination of selective serotonin reuptake inhibitors

“…Of the different methods developed for enantioseparation of (±)‐ trans ‐Pxn and the determination of (−)‐ and (+)‐ trans ‐Pxn contents, using different CSPs, some are selective, precise, accurate and offer good recovery. The method reported by Lisowska‐Kuźmicz et al () shows that (+)‐ trans ‐Pxn [as compared with (−)‐enantiomer] forms a more stable solute stationary phase complex on ovomucoid than on amylose tris(3,5‐dimethylphenyl)carbamate stationary phase; the amount of (+)‐ trans ‐Pxn enantiomer was ≥0.01% under the analysis conditions.…”

“…Enantioseparation and determination of (−)‐ trans ‐Pxn and (+)‐ trans ‐Pxn from the commercial tablets was achieved (Lisowska‐Kuźmicz et al, ) using a column of (a) aminopropylsilane silica derivatized with ovomucoid and 10 m m phosphate buffer (pH adjusted to 3.5 with concentrated H 3 PO 4 or 1 m KOH)–acetonitrile (98:2, v/v) as the mobile phase at a flow rate of 1.5 ml min −1 and UV detection (at 295 nm), and (b) a silica‐based amylose tris(3,5‐dimethylphenyl)carbamate (Chiralpak AD‐H) column with n ‐hexane–ethanol–ethanolamine (80:20:0.2, v/v), as the mobile phase at a flow rate 1 ml min −1 and UV detection at 295 nm. Resolution was 2.60 in both cases; the (−)‐enantiomer eluted before (+)‐enantiomer on (a) while the (+)‐enantiomer eluted before (−)‐enantiomer on (b).…”

“…In 2016, the elution sequences of the enantiomers of transparoxetine were investigated on two pairs of pseudo-enantiomeric CSPs based on chiral zwitterionic Cinchona alkaloids fused with (R,R)or (S,S)-trans-2-aminocyclohexanesulfonic acid using MeOH-Tetrahydrofuran (THF), MeCN-THF, MeCN-THF-water and MeOH-MeCN-THF containing organic acid and base additives as the polarionic or hydro-organic mobile phases; the results were used to gain an insight into the underlying molecular recognition events between the chiral selectors and the analyte enantiomers(Grecsó et al, 2016).Of the different methods developed for enantioseparation of (±)trans-Pxn and the determination of (−)-and (+)-trans-Pxn contents, using different CSPs, some are selective, precise, accurate and offer good recovery. The method reported byLisowska-Kuźmicz et al (2014) shows that (+)-trans-Pxn [as compared with (−)-enantiomer] forms a more stable solute stationary phase complex on ovomucoid than on amylose tris(3,5-dimethylphenyl)carbamate stationary phase; the amount of (+)-trans-Pxn enantiomer was ≥0.01% under the analysis conditions.…”