Passa al contenuto
Merck

Isolation of oxidative degradation products of atorvastatin with supercritical fluid chromatography.

Biomedical chromatography : BMC (2015-05-27)
Slavko Klobčar, Helena Prosen
ABSTRACT

The isolation of four oxidative degradation products of atorvastatin using preparative high-performance liquid chromatography applying at least two chromatographic steps is known from the literature. In this paper it is shown that the same four impurities could be isolated from similarly prepared mixtures in only one step using supercritical fluid chromatography. The methods for separation were developed and optimized. The preparation of the mixtures was altered in such a way as to enhance the concentration of desired impurities. Appropriate solvents were applied for collection of separated impurities in order to prevent degradation. The structures of the isolated impurities were confirmed and their purity determined. The preparative supercritical fluid chromatography has proven to be superior to preparative HPLC regarding achieved purity of standards applying fewer chromatographic as well as isolation steps.

MATERIALI
N° Catalogo
Marchio
Descrizione del prodotto

Sigma-Aldrich
Acido trifluoroacetico, ReagentPlus®, 99%
Sigma-Aldrich
Metanolo, ACS reagent, ≥99.8%
Sigma-Aldrich
N,N-dimetilformammide, ACS reagent, ≥99.8%
Sigma-Aldrich
Acetonitrile, anhydrous, 99.8%
Sigma-Aldrich
Acetonitrile, ACS reagent, ≥99.5%
Sigma-Aldrich
N,N-dimetilformammide, anhydrous, 99.8%
Sigma-Aldrich
Acido trifluoroacetico, puriss. p.a., suitable for HPLC, ≥99.0% (GC)
Sigma-Aldrich
Metanolo, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
Sigma-Aldrich
Metanolo, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Trietilammina, ≥99.5%
Sigma-Aldrich
Metanolo, anhydrous, 99.8%
Sigma-Aldrich
N,N-dimetilformammide, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥99.8% (GC)
Sigma-Aldrich
Acido trifluoroacetico, ≥99%, for protein sequencing
Sigma-Aldrich
N,N-dimetilformammide, ReagentPlus®, ≥99%
Sigma-Aldrich
N,N-dimetilformammide, for molecular biology, ≥99%
Sigma-Aldrich
Metanolo, BioReagent, ≥99.93%
Sigma-Aldrich
Metanolo, Absolute - Acetone free
Sigma-Aldrich
Metanolo, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Trietilammina, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
N,N-dimetilformammide, biotech. grade, ≥99.9%
Sigma-Aldrich
Trietilammina, ≥99%
Sigma-Aldrich
Metanolo, ACS reagent, ≥99.8%
Sigma-Aldrich
Acetonitrile, biotech. grade, ≥99.93%
Sigma-Aldrich
Trietilammina, puriss. p.a., ≥99.5% (GC)
Sigma-Aldrich
Benzamide, 99%
Sigma-Aldrich
Metanolo, ACS reagent, ≥99.8%
Sigma-Aldrich
Acetonitrile, ReagentPlus®, 99%
Sigma-Aldrich
Metanolo, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)
Sigma-Aldrich
Acetonitrile, electronic grade, 99.999% trace metals basis
Sigma-Aldrich
Trietilammina, for amino acid analysis, ≥99.5% (GC)