Skip to Content
Merck
  • Development of a purity control strategy for pemetrexed disodium and validation of associated analytical methodology.

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
ABSTRACT

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.

MATERIALS
Product Number
Brand
Product Description

Supelco
Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetic acid, glacial, ACS reagent, ≥99.7%
Sigma-Aldrich
Acetic acid, glacial, ≥99.99% trace metals basis
Sigma-Aldrich
Acetic acid, glacial, puriss., 99-100%
Sigma-Aldrich
Acetic acid, 99.5-100.0%
Sigma-Aldrich
Acetic acid, ≥99.7%, for titration in non-aqueous medium
Sigma-Aldrich
Acetic acid, ≥99.7%, SAJ super special grade
Sigma-Aldrich
Acetic acid solution, 1 M, 1 N
Sigma-Aldrich
Acetic acid, ≥99.7%
Sigma-Aldrich
Acetic acid solution, SAJ first grade, 27.0-33.0%
Sigma-Aldrich
Acetic acid, JIS special grade, ≥99.7%
Sigma-Aldrich
Acetic acid, SAJ first grade, ≥99.0%
Sigma-Aldrich
Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
Supelco
Acetic acid, analytical standard
Sigma-Aldrich
Acetic acid, ≥99.5%, FCC, FG
Sigma-Aldrich
Acetic acid, glacial, ReagentPlus®, ≥99%
Supelco
Sodium hydroxide solution, 49-51% in water, eluent for IC
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 5 % (v/v) water, 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Acetic acid, natural, ≥99.5%, FG
Sigma-Aldrich
Acetonitrile-d3, "100%", 99.96 atom % D
Sigma-Aldrich
Sodium hydroxide, BioUltra, for luminescence, ≥98.0% (T), pellets
Sigma-Aldrich
Acetonitrile-d3, 99.8 atom % D, contains 0.03 % (v/v) TMS
Sigma-Aldrich
Sodium hydroxide solution, 0.05 M
Sigma-Aldrich
Sodium hydroxide solution, 0.1 M
Sigma-Aldrich
Sodium hydroxide solution, 7 M
Sigma-Aldrich
Sodium hydroxide solution, 0.5 M