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
Acetic acid, analytical standard
Sigma-Aldrich
Acetonitrile-d3, 96-97 atom % D, D2O 15-20 %
Millipore
Hydrogen peroxide solution, 3%, suitable for microbiology
Sigma-Aldrich
Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)
Sigma-Aldrich
Acetic acid, natural, ≥99.5%, FG
Sigma-Aldrich
Acetic acid, ≥99.5%, FCC, FG
Sigma-Aldrich
Ammonium formate, ≥99.995% trace metals basis
Sigma-Aldrich
Acetonitrile-d3, "100%", 99.96 atom % D
Supelco
Ammonium formate, eluent additive for LC-MS, LiChropur, ≥99.0%
Sigma-Aldrich
Acetonitrile-d3, ≥99.8 atom % D, anhydrous
Sigma-Aldrich
Acetonitrile-d3, 99.8 atom % D, contains 0.03 % (v/v) TMS
Sigma-Aldrich
Acetonitrile-d3, 99.8 atom % D, contains 1 % (v/v) TMS
Sigma-Aldrich
Acetic acid, 99.5-100.0%
Sigma-Aldrich
Acetic acid, SAJ first grade, ≥99.0%
Sigma-Aldrich
Acetic acid, ≥99.7%, for titration in non-aqueous medium
Sigma-Aldrich
Acetic acid, JIS special grade, ≥99.7%
Sigma-Aldrich
Acetic acid, ≥99.7%
Sigma-Aldrich
Hydrogen peroxide solution, JIS special grade, 30.0-35.5%
Sigma-Aldrich
Acetic acid solution, SAJ first grade, 27.0-33.0%
Sigma-Aldrich
Hydrogen peroxide solution, SAJ first grade, ≥30.0%
Sigma-Aldrich
Acetic acid, ≥99.7%, SAJ super special grade
Sigma-Aldrich
Acetic acid solution, 1 M, 1 N
Sigma-Aldrich
Ammonium formate, SAJ first grade, ≥95.0%
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-12C2, 99.9 atom % 12C
Sigma-Aldrich
Sodium hydroxide, BioXtra, ≥98% (acidimetric), pellets (anhydrous)
Sigma-Aldrich
Sodium hydroxide, puriss., meets analytical specification of Ph. Eur., BP, NF, E524, 98-100.5%, pellets
Sigma-Aldrich
Sodium hydroxide, reagent grade, ≥98%, pellets (anhydrous)
Sigma-Aldrich
Sodium hydroxide, reagent grade, 97%, flakes