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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
RESUMEN

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.

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Acetonitrilo, suitable for HPLC, gradient grade, ≥99.9%
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Ácido acético, glacial, ACS reagent, ≥99.7%
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Acetonitrilo, HPLC Plus, ≥99.9%
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Hidróxido de sodio, ACS reagent, ≥97.0%, pellets
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Peróxido de hidrógeno solution, contains inhibitor, 30 wt. % in H2O, ACS reagent
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Ácido acético, glacial, ReagentPlus®, ≥99%
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Hidróxido de sodio, reagent grade, ≥98%, pellets (anhydrous)
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Hidróxido de sodio solution, 50% in H2O
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Peróxido de hidrógeno solution, 30 % (w/w) in H2O, contains stabilizer
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Acetonitrilo-d3, ≥99.8 atom % D
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Ácido fórmico, ACS reagent, ≥96%
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Ácido fórmico, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%
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Peróxido de hidrógeno solution, 50 wt. % in H2O, stabilized
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Acetonitrilo, anhydrous, 99.8%
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Ácido acético solution, suitable for HPLC
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Ácido fórmico, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
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