A stability-indicating, ion-pairing, reversed-phase liquid chromatography method for studies of daunorubicin degradation in i.v. infusion fluids

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Abstract

A new stability-indicating method based on high-performance liquid chromatography coupled to ultraviolet and evaporative light scattering detection (HPLC-UV-ELSD) was developed for the quantification of daunorubicin. This is an ion-pairing, reversed-phase method. The column was a Synergi MAX-RP C12 4 μm (150 mm × 4.6 mm). The mobile phase was 6.2 mM nonafluoropentanoic acid in aqueous solution and acetonitrile under isocratic elution mode. The drug was subjected to oxidation, basic and acid hydrolysis to apply stress conditions. Good resolution was achieved between daunorubicin, related products and all degradation products in an overall analytical run time of approximately 16 min with the parent compound daunorubicin eluting at approximately 8 min. The method was fully validated according to ICH guidelines and SFSTP protocols in terms of accuracy, precision, specificity and linearity. For daunorubicin, the decision criteria selected consisted of the acceptability limits (±3%) and the proportion of results within the calculated tolerance intervals (95%). In conclusion, the proposed analytical procedures were validated over the selected validation domains daunorubicin (0.25–0.45 mg/mL) and shown to provide a very effective method. Physical and chemical stability study was carried out on daunorubicin preparation in our hospital centralized pharmacy unit.

Graphical abstract

HPLC analysis of a solution of daunorubicin (0.4 mg/mL) with different chromatographic conditions: (A) Column: Synergi MAX-RP C12 4 μm (150 mm × 4.6 mm I.D.). Isocratic elution: 10 mM acid acetic buffer (pH 4.8) and acetonitrile (62:38, v/v). (B) Column: Polar-RP column 4 μm (150 mm × 4.6 mm I.D.). Isocratic elution: 6.2 mM NFPA in water and acetonitrile (65:35, v/v). (C) Column: Synergi MAX-RP C12 4 μm (150 mm × 4.6 mm I.D.). Isocratic elution: 6.2 mM NFPA in water and acetonitrile (65:35, v/v). Flow rate: 1 mL min−1; injection volume: 20 μL; UV detection at 254 nm.

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