title: Direct separation of the enantiomers of oxaliplatin on a cellulose-based chiral stationary phase in hydrophilic interaction liquid chromatography mode.
abstract: (R,R)-oxaliplatin is an anticancer enantiopure active pharmaceutical ingredient. Little attention has been devoted to the analysis of its enantiomeric composition. The enantioselective HPLC method reported in the current Pharmacopoeias shows clear disadvantages with regard to the low resolution and long elution times. In this work, it has been proven the applicability of a last generation polysaccharide-based chiral stationary phase (CSP), i.e. the Chiralpak IC-3, in the enantioseparation of oxaliplatin. Experimental results demonstrated the benefits arising from the development of enantioselective hydrophilic interaction liquid chromatography (HILIC) based strategies. A baseline separation with resolution factor of 5.8 was achieved using a 100mm×4.6mm I.D. IC-3 column set at the temperature of 40°C and a mobile phase consisting of acetonitrile-water 100:5 mixture. At a flow rate of 1mLmin(-1) the separation was completed within 8min. The optimized method was proven to be sensitive with LOD and LOQ of the enantiomeric impurity of 0.07 and 0.21μgmL(-1), respectively.
authors.affiliation: Istituto Superiore di Sanità, Dipartimento del Farmaco, Viale Regina Elena 299, I-00161 Rome, Italy.
authors.forename: Bruno
authors.initials: B
authors.lastname: Gallinella
authors.affiliation: Istituto Superiore di Sanità, Dipartimento del Farmaco, Viale Regina Elena 299, I-00161 Rome, Italy.
authors.forename: Lucia
authors.initials: L
authors.lastname: Bucciarelli
authors.affiliation: Istituto Superiore di Sanità, Dipartimento del Farmaco, Viale Regina Elena 299, I-00161 Rome, Italy.
authors.forename: Leo
authors.initials: L
authors.lastname: Zanitti
authors.affiliation: Istituto Superiore di Sanità, Dipartimento del Farmaco, Viale Regina Elena 299, I-00161 Rome, Italy.
authors.forename: Rosella
authors.initials: R
authors.lastname: Ferretti
authors.affiliation: Istituto Superiore di Sanità, Dipartimento del Farmaco, Viale Regina Elena 299, I-00161 Rome, Italy. Electronic address: rcirilli@iss.it.
authors.forename: Roberto
authors.initials: R
authors.lastname: Cirilli
mesh_terms: D000970:Antineoplastic Agents / Q000302:isolation & purification*; D002219:Carbamates; D002482:Cellulose / Q000031:analogs & derivatives*; D002853:Chromatography, Liquid / Q000379:methods; D057927:Hydrophobic and Hydrophilic Interactions; D009944:Organoplatinum Compounds / Q000302:isolation & purification*; D000077150:Oxaliplatin; D013237:Stereoisomerism; D013696:Temperature
chemical_list: D000970:Antineoplastic Agents; D002219:Carbamates; D009944:Organoplatinum Compounds; D000077150:Oxaliplatin; D002482:Cellulose
keywords: Anticancer drug; Chiralpak IC-3; Enantiomer separation; HILIC; Oxaliplatin; Temperature effects