Accéder au contenu
Merck

Development of a purity control strategy for pemetrexed disodium and validation of associated analytical methodology.

Journal of pharmaceutical and biomedical analysis (2014-12-22)
Anne Warner, Irina Piraner, Heather Weimer, Kevin White
RÉSUMÉ

Stability-indicating reversed phase HPLC methods have been developed and validated for the determination of 13 potential process and degradation impurities in pemetrexed disodium drug substance (DS) and pemetrexed for injection drug product (DP). This paper describes the development of HPLC-UV impurity methods for drug substance and drug product. Relative response factors (RRF) have been determined using HPLC-UV in tandem with CAD or by NMR detection. Conditions for the generation of system suitability solutions are described and assure adequate chromatographic resolution and peak identification without the need for impurity reference standards. The methods were fully validated and demonstrated to have acceptable specificity, linearity, accuracy, repeatability, intermediate precision, detection/quantitation limit, and robustness.

MATÉRIAUX
Référence du produit
Marque
Description du produit

Sigma-Aldrich
Acétonitrile, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Acide acétique, glacial, ACS reagent, ≥99.7%
Sigma-Aldrich
Acétonitrile, HPLC Plus, ≥99.9%
Sigma-Aldrich
Hydroxyde de sodium, ACS reagent, ≥97.0%, pellets
Sigma-Aldrich
Peroxyde d'hydrogène solution, contains inhibitor, 30 wt. % in H2O, ACS reagent
Sigma-Aldrich
Acide acétique, glacial, ReagentPlus®, ≥99%
Sigma-Aldrich
Hydroxyde de sodium, reagent grade, ≥98%, pellets (anhydrous)
Sigma-Aldrich
Acide formique, reagent grade, ≥95%
Sigma-Aldrich
Hydroxyde de sodium solution, 50% in H2O
Sigma-Aldrich
Peroxyde d'hydrogène solution, 30 % (w/w) in H2O, contains stabilizer
Sigma-Aldrich
Acétonitrile-d3, ≥99.8 atom % D
Sigma-Aldrich
Acide formique, ACS reagent, ≥96%
Sigma-Aldrich
Acétonitrile, anhydrous, 99.8%
Sigma-Aldrich
Acétonitrile, ACS reagent, ≥99.5%
Sigma-Aldrich
Hydroxyde de sodium solution, BioUltra, for molecular biology, 10 M in H2O
Sigma-Aldrich
Formate d′ammonium, reagent grade, 97%
Sigma-Aldrich
Peroxyde d'hydrogène solution, 50 wt. % in H2O, stabilized
Sigma-Aldrich
Acétonitrile, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Acide acétique, glacial, ≥99.99% trace metals basis
Sigma-Aldrich
Hydroxyde de sodium solution, 1.0 N, BioReagent, suitable for cell culture
Sigma-Aldrich
Hydroxyde de sodium, BioXtra, ≥98% (acidimetric), pellets (anhydrous)
Sigma-Aldrich
Acide acétique solution, suitable for HPLC
Sigma-Aldrich
Hydroxyde de sodium, reagent grade, 97%, powder
Supelco
Formate d′ammonium, eluent additive for LC-MS, LiChropur, ≥99.0%
Sigma-Aldrich
Hydroxyde de sodium, puriss., meets analytical specification of Ph. Eur., BP, NF, E524, 98-100.5%, pellets
Sigma-Aldrich
Formate d′ammonium, ≥99.995% trace metals basis
Sigma-Aldrich
Acide formique, ACS reagent, ≥88%
Sigma-Aldrich
Hydroxyde de sodium, pellets, semiconductor grade, 99.99% trace metals basis
Sigma-Aldrich
Hydroxyde de sodium solution, 5.0 M
Sigma-Aldrich
Ammonium formate solution, BioUltra, 10 M in H2O