Validated Chiral LC Method for the Enantiomeric Separation of Palonosetron Hydrochloride

Radhakrishnanand, P.; Rao, D. V. Subba; Himabindu, V.

doi:10.1365/s10337-008-0887-9

Cited by 12 publications

(11 citation statements)

References 7 publications

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“…The interactions of other two enantiomers PALO (3aS, 2R), and PALO (3aR, 2S) have not been considered. It was observed that under the same experimental conditions as reported in the literature [8] PALO (3aS, 2R) isomer was eluted with PALO (3aR, 2R) isomer. So it is not a suitable method for quantifying the enantiomers in the real samples.…”

Section: Introductionsupporting

confidence: 78%

Section: Specificity and Mass Balance Studysupporting

confidence: 62%

“…Due to free solubility of PALO in polar solvent, the first experiment was conducted with a mobile phase composition of hexane: ethanol: trifluoroacetic acid: diethyl amine (90:10:0.5:2, v/v) with Chiralcel OD-H column. The trifluoroacetic acid and diethyl amine were used as additive with mobile phase as reported in the literature [8]. But three impurities (comp 2, 3, and 4) were eluted at the same retention time.…”

Section: Methods Development and Optimization Of Chromatographic Condimentioning

confidence: 99%

“…So far, to our knowledge no chiral liquid chromatographic method on enantiomeric separation of four enantiomers of PALO is reported in the literature. One chiral LC method for the separation of PALO enantiomers has been reported by Radhakrishnanand et al [8]. The major drawback of this method is that it has been used to separate only PALO (3aS, 2S) from its enantiomer (3aR, 2R).…”

Section: Introductionmentioning

confidence: 99%

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Enantioseparation of Palonosetron Hydrochloride and Its Related Enantiomeric Impurities by Computer Simulation and Validation

Murthy¹,

Krishnaiah²,

Jyothirmayi³

et al. 2011

AJAC

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A rapid, simple and single stereo selective high-performance liquid chromatographic (HPLC) method was developed and validated for enantiomers of palonosetron hydrochloride (PALO) and its process related chiral impurities. A computer simulating software was used for the development of chiral method. The developed method was able to separate not only the enantiomers of palonosetron hydrochloride but also its process related chiral impurities within 12 min. The chromatographic separation was carried out by normal phase chromatography using a 3 µm column of cellulose based chiral stationary phase (Chiralcel-OD 250mm × 4.6mm) with a mobile phase comprised of n-hexane: ethanol: methanol: heptafluoro butyric acid: diethyl amine (70:15:15:0.05:0.1, v/v) at a flow rate of 1.0 mL/min. The effects of additive concentration as well as nature of polar organic modifier, flow rate, and temperature on enantioselectivity were investigated. The limit of detection (LOD) and limit of quantification (LOQ) of the palonosetron isomers and its related chiral impurities were found to be in the range 0.06-0.10 µg/mL and 0.14 -0.24 µg/mL respectively. The method showed excellent linearity (R 2 > 0.998) over a range of 0.14 to 1.125 µg/mL. The percentage recovery of the isomers in bulk drug samples ranged from 87.0 to 116.0.

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Section: Introductionsupporting

confidence: 78%

Section: Specificity and Mass Balance Studysupporting

confidence: 62%

Section: Methods Development and Optimization Of Chromatographic Condimentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Enantioseparation of Palonosetron Hydrochloride and Its Related Enantiomeric Impurities by Computer Simulation and Validation

Murthy¹,

Krishnaiah²,

Jyothirmayi³

et al. 2011

AJAC

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show abstract

“…Some analytical methods for the enantiomeric separation of PALO stereoisomers by HPLC and CE have been developed. Radhakrishnanand et al [7] reported a chiral HPLC method for the separation of PALO enantiomers, using a CHIRALPAK IC column and a mobile phase containing n-hexane, ethanol, 1,4-dioxane, trifluoroacetic acid, and diethylamine in a ratio of 65:30:5:0.3: 0.3 v/v. The major drawback of this method is that it only separates PALO (3aS, 2S) from its enantiomer PALO (3aR, 2R).…”

Section: Introductionmentioning

confidence: 99%

Solvent‐modified MEKC for the enantioseparation of palonosetron hydrochloride and related enantiomeric impurities

Shi

et al. 2015

Electrophoresis

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The effect of ten water-soluble organic solvents on MEKC separation of palonosetron hydrochloride (PALO) stereoisomers using sodium cholate (SC) as chiral selector has been studied. The first chiral CE method fit for the analysis of unwanted PALO distomers (enantiomeric impurities) of low concentrations in the presence of high concentration of the main eutomer has been developed, based on solvent-modified MEKC mode. It was found that methanol provides the best separation among the solvents tested. And an SC concentration of 30 mM is proper to provide good resolutions in shorter time and adequate sample capacity, instead of 70 mM as previously reported. The developed method can be used to analyze unwanted PALO distomers of a few micrograms per milliliter in the presence of the main eutomer with a concentration as high as 1.0 mg/mL.

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Separation of palonosetron stereoisomers by electrokinetic chromatography using sodium cholate as chiral selector: Comparison of separation modes and elucidation of migration orders

Yang

Shi

et al. 2013

Electrophoresis

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Based on sodium cholate as chiral selector, four stereoisomers of palonosetron hydrochloride, i.e. PALO (3aS, 2S), PALO (3aR, 2R), PALO (3aS, 2R), and PALO (3aR, 2S), have been separated by five EKC modes, i.e. MEKC, solvent-modified MEKC, cosurfactant-modified MEKC, MEEKC, and MEEKC without cosurfactant. The performances of different modes were compared. The migration order and its change with experimental conditions were elucidated. In every mode studied, the migration orders in each enantiomeric pair were (3aS, 2S), (3aR, 2R) and (3aS, 2R), (3aR, 2S), respectively, determined by the selectivity of chiral selector (chromatographic mechanism). Enantiomeric pair (3aS, 2S), (3aR, 2R) was eluted before enantiomeric pair (3aS, 2R), (3aR, 2S) due to mobility difference (electrophoretic mechanism). For the separation between (3aR, 2R) and (3aS, 2R), the second enantiomer of the first pair and the first enantiomer of the second pair, two mechanisms gave opposite migration orders according to the measured selectivity and mobility data. Therefore, three different migration orders were observed at different conditions, depending on the relative strength of two effects.

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Validated Chiral LC Method for the Enantiomeric Separation of Palonosetron Hydrochloride

Cited by 12 publications

References 7 publications

Enantioseparation of Palonosetron Hydrochloride and Its Related Enantiomeric Impurities by Computer Simulation and Validation

Enantioseparation of Palonosetron Hydrochloride and Its Related Enantiomeric Impurities by Computer Simulation and Validation

Solvent‐modified MEKC for the enantioseparation of palonosetron hydrochloride and related enantiomeric impurities

Separation of palonosetron stereoisomers by electrokinetic chromatography using sodium cholate as chiral selector: Comparison of separation modes and elucidation of migration orders

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