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  • 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
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
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Acetic acid, JIS special grade, ≥99.7%
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Acetic acid solution, 1 M, 1 N
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Acetic acid, SAJ first grade, ≥99.0%
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Sodium hydroxide solution, 6 M
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Acetic acid, ≥99.7%
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Sodium hydroxide solution, 0.1 M
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Sodium hydroxide solution, 1 M
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Sodium hydroxide, JIS special grade, ≥96.0%
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Ammonium formate, SAJ first grade, ≥95.0%
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Hydrogen peroxide solution, SAJ first grade, ≥30.0%
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Acetic acid, ≥99.7%, suitable for amino acid analysis
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Acetic acid-12C2, 99.9 atom % 12C
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Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 5 % (v/v) water, 0.1 % (v/v) formic acid, suitable for HPLC
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Hydrogen peroxide solution, ≥30%, for trace analysis
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Hydrogen peroxide solution, tested according to Ph. Eur.
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Ammonium formate, ≥99.995% trace metals basis
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Acetonitrile-d3, 96-97 atom % D, D2O 15-20 %
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