Demonstrative validation study employing a packed column pressurized fluid chromatography method that provides assay, achiral impurities, chiral impurity, and IR identity testing for a drug substance.

M Ashraf-Khorassani; L T Taylor; D G Williams; D A Roston; T T Catalano

doi:10.1016/s0731-7085(01)00441-1

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PubMed · 11600285

Demonstrative validation study employing a packed column pressurized fluid chromatography method that provides assay, achiral impurities, chiral impurity, and IR identity testing for a drug substance.

M Ashraf-Khorassani·L T Taylor·D G Williams·D A Roston·T T Catalano

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Abstract

Assay development, assay validation, and documentation are reported here for a single packed column pressurized fluid chromatographic/ultraviolet (UV) method that provides: (1) simultaneous detection and quantification for the chiral drug, the chiral impurity and seven achiral impurities; and (2) a Fourier transform infrared (FT-IR) spectrometric identification test result for the Searle drug substance sample, xemilofiban. The separation is achieved in less than 30 min with three columns in tandem and a gradient of CO2-CH3OH. The post-column flow is split between UV (assay) and FT-IR (identification). Precision and accuracy are consistent within figures of merit obtained by liquid chromatographic-ultraviolet assays on analogous drug substances. The reported procedure combines three typical drug substance tests into one test (e.g. chiral impurities, achiral impurities, and infrared identification).

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Chromatography, Liquid Drug Contamination Pharmaceutical Preparations Reproducibility of Results Solutions Spectrophotometry, Ultraviolet Spectroscopy, Fourier Transform Infrared Journal Article Validation Study

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M Ashraf-Khorassani, L T Taylor, D G Williams, D A Roston, T T Catalano. 2001. Demonstrative validation study employing a packed column pressurized fluid chromatography method that provides assay, achiral impurities, chiral impurity, and IR identity testing for a drug substance.. https://doi.org/10.1016/s0731-7085(01)00441-1

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