Determination of diminazene aceturate in pharmaceutical formulations by HPLC and identification of related substances by lC/MS

C. Atsriku, D.G. Watson, J.N.A. Tettey, M.H. Grant, G.G. Skellern

Research output: Contribution to journalArticle

25 Citations (Scopus)

Abstract

A validated, reversed-phase, isocratic high-performance liquid chromatographic method for the simultaneous assay of diminazene aceturate, antipyrine (excipient) and diminazene impurities in pharmaceutical formulations is described. The chromatographic system consisted of a Lichrospher-60 RP-select B column with a mobile phase composition of acetonitrile–methanol–ammonium formate (pH 4.0, 20 mM) (10:10: 80 v/v/v) and UV detection at 254 nm. The method is specific, precise and accurate for the determination of diminazene in the presence of its manufacturing and degradation impurities with a limit of detection and quantification of 50 ng/ml and 10 μg/ml (RSD<3.0%), respectively. The major manufacturing impurity [1-(4 amidino phenyl)3-(4 carbamoyl phenyl)-triazene] and a degradant (p-aminobenzamidine) of diminazene aceturate have been resolved and identified by liquid chromatography/electrospray ionization-mass spectrometry operated in a positive ion mode.
LanguageEnglish
Pages979-986
Number of pages8
JournalJournal of Pharmaceutical and Biomedical Analysis
Volume30
Issue number4
DOIs
Publication statusPublished - 2002

Fingerprint

Diminazene
Drug Compounding
formic acid
Triazenes
High Pressure Liquid Chromatography
Impurities
Antipyrine
Electrospray Ionization Mass Spectrometry
Excipients
Liquid Chromatography
Pharmaceutical Preparations
Methanol
Limit of Detection
Electrospray ionization
Liquid chromatography
Ions
Phase composition
Mass spectrometry
Assays
Positive ions

Keywords

  • diminazene aceturate
  • HPLC
  • pharmaceutical formulations
  • spectrometry

Cite this

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title = "Determination of diminazene aceturate in pharmaceutical formulations by HPLC and identification of related substances by lC/MS",
abstract = "A validated, reversed-phase, isocratic high-performance liquid chromatographic method for the simultaneous assay of diminazene aceturate, antipyrine (excipient) and diminazene impurities in pharmaceutical formulations is described. The chromatographic system consisted of a Lichrospher-60 RP-select B column with a mobile phase composition of acetonitrile–methanol–ammonium formate (pH 4.0, 20 mM) (10:10: 80 v/v/v) and UV detection at 254 nm. The method is specific, precise and accurate for the determination of diminazene in the presence of its manufacturing and degradation impurities with a limit of detection and quantification of 50 ng/ml and 10 μg/ml (RSD<3.0{\%}), respectively. The major manufacturing impurity [1-(4 amidino phenyl)3-(4 carbamoyl phenyl)-triazene] and a degradant (p-aminobenzamidine) of diminazene aceturate have been resolved and identified by liquid chromatography/electrospray ionization-mass spectrometry operated in a positive ion mode.",
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Determination of diminazene aceturate in pharmaceutical formulations by HPLC and identification of related substances by lC/MS. / Atsriku, C.; Watson, D.G.; Tettey, J.N.A.; Grant, M.H.; Skellern, G.G.

In: Journal of Pharmaceutical and Biomedical Analysis, Vol. 30, No. 4, 2002, p. 979-986.

Research output: Contribution to journalArticle

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T1 - Determination of diminazene aceturate in pharmaceutical formulations by HPLC and identification of related substances by lC/MS

AU - Atsriku, C.

AU - Watson, D.G.

AU - Tettey, J.N.A.

AU - Grant, M.H.

AU - Skellern, G.G.

PY - 2002

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AB - A validated, reversed-phase, isocratic high-performance liquid chromatographic method for the simultaneous assay of diminazene aceturate, antipyrine (excipient) and diminazene impurities in pharmaceutical formulations is described. The chromatographic system consisted of a Lichrospher-60 RP-select B column with a mobile phase composition of acetonitrile–methanol–ammonium formate (pH 4.0, 20 mM) (10:10: 80 v/v/v) and UV detection at 254 nm. The method is specific, precise and accurate for the determination of diminazene in the presence of its manufacturing and degradation impurities with a limit of detection and quantification of 50 ng/ml and 10 μg/ml (RSD<3.0%), respectively. The major manufacturing impurity [1-(4 amidino phenyl)3-(4 carbamoyl phenyl)-triazene] and a degradant (p-aminobenzamidine) of diminazene aceturate have been resolved and identified by liquid chromatography/electrospray ionization-mass spectrometry operated in a positive ion mode.

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