Identification of gentamicin impurities by liquid chromatography tandem mass spectrometry

Grahek, Rok; Zupančič‐Kralj, Lucija

doi:10.1016/j.jpba.2009.06.004

Cited by 41 publications

(34 citation statements)

References 28 publications

(45 reference statements)

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“…A volatile mobile phase with TFA at pH 2.4 adjusted with ammonia and a gradient with methanol were used to separate and detect impurities in gentamicin bulk samples with electrospray ionization (ESI) and ion trap mass spectrometry. Recently Grahek and Zupančič-Kralj [7] reported a gradient LC-MS method using a volatile mobile phase containing TFA and methanol. Seventeen impurities were detected and identified in a gentamicin sample with an atmospheric pressure chemical ionization (APCI) probe.…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Mass spectrometric characterization of gentamicin components separated by the new European Pharmacopoeia method

Li¹,

Schepdael²,

Hoogmartens³

et al. 2011

Journal of Pharmaceutical and Biomedical Analysis

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Section: Introductionmentioning

confidence: 99%

“…Thus, fractions containing the peaks of interest were collected, desalted and introduced in the MS. The results were also compared with those of previously published LC-MS methods using a volatile mobile phase [6,7].…”

Section: Introductionmentioning

confidence: 99%

Mass spectrometric characterization of gentamicin components separated by the new European Pharmacopoeia method

Li¹,

Schepdael²,

Hoogmartens³

et al. 2011

Journal of Pharmaceutical and Biomedical Analysis

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“…Many separation methods have been reported in literature for the determination of gentamicin compounds, such as thin layer, paper chromatography, craig distribution, ion exchange liquid chromatography, reversed phase liquid chromatography and capillary electrophoresis . Much effort has been paid to the detection techniques, such as refractive index (RI) detection [21,35], evaporative light scattering detection (ELSD) [29,30], pre-column derivatization followed by UV detection [36,37], pulse electrochemical detection (PED) [16,24,31,49], charged aerosol detection (CAD) [39] and mass spectrometry (MS) [33,38]. Pre-column derivatization, RI and ELSD detection have shortcomings for analysis of gentamicin like sensitivi- ty and efficiency [40].…”

Section: Introductionmentioning

confidence: 99%

Impurity analysis of gentamicin bulk samples by improved liquid chromatography-ion trap mass spectrometry

Zheng

Wang

et al. 2011

Sci. China Chem.

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Several gentamicin bulk samples from different origins were investigated using an LC/MS method. LC equipped with ion trap MS with positive ionization was performed on a Capcell Pak C 18 (AQ) column with the mobile phase containing 50 mM trifluoroacetic (TFA) and methanol. Impurities present in batches of gentamicin bulk samples were elucidated and compared according to their fragmentation behavior. In total seventeen impurities present in samples, five impurities were not elucidated and two compounds were identified preliminarily. It was observed that the impurity profiles were different in samples from different origins which indicate necessity in the quality control of gentamicin. gentamicin, liquid chromatography, LC/MS, impurity analysis

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“…Gentamicin usually contains several components with different structures at given ratio [15]. Main components were identified as gentamicins C1a, C2, C2a and C1 by LC/ MS analysis [15].…”

Section: Resultsmentioning

confidence: 99%

Preparative purification of gentamicin components using high‐speed counter‐current chromatography coupled with electrospray mass spectrometry

Inoue

Hattori

Horie

et al. 2011

J of Separation Science

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We developed a useful and preparative method based on high-speed counter-current chromatography with mass spectrometry (HSCCC/MS) to purify gentamicin C1a, C2/2a and C1 from standard powder. The analytes were purified on the HSCCC model CCC-1000 (multi-layer coil planet centrifuge) with a volatile two-phase solvent system composed of n-butanol/10% aqueous ammonia solution (50:50, v/v) and detected on an LCMS-2020EV quadrupole mass spectrometer fitted with an electrospray ionization (ESI) source system in positive ionization following scan mode (m/z 100-500). The HSCCC/ESI-MS peaks indicated that gentamicin C1a (m/z 450: [M+H](+)), C2/2a (m/z 464: [M+H](+)) and C1 (m/z 478: [M+H](+)) have the peak resolution values of 1.3 and 1.7 from 30 mg of loaded gentamicin powder. The HSCCC yielded 3.9 mg of gentamicin C1a, 12.6 mg of gentamicin C2/2a and 12.0 mg of gentamicin C1. These purified substances were analyzed by LC/MS with scan positive-mode. Based on the LC/MS chromatograms and spectra of the fractions, analytes were estimated to be over 95% pure. These gentamicin isomers of C1a, C2/2a and C1 were evaluated for their antibacterial activities. The overall results indicate that this approach of HSCCC/MS is a powerful technique for the purification of gentamicin components.

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Identification of gentamicin impurities by liquid chromatography tandem mass spectrometry

Cited by 41 publications

References 28 publications

Mass spectrometric characterization of gentamicin components separated by the new European Pharmacopoeia method

Mass spectrometric characterization of gentamicin components separated by the new European Pharmacopoeia method

Impurity analysis of gentamicin bulk samples by improved liquid chromatography-ion trap mass spectrometry

Preparative purification of gentamicin components using high‐speed counter‐current chromatography coupled with electrospray mass spectrometry

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