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

Zheng, Chao; Wang, Bochu; Wang, Ming-juan; Hoogmartens, Jos; Schepdael, Ann Van; Adams, Erwin

doi:10.1007/s11426-011-4304-0

Cited by 3 publications

(4 citation statements)

References 41 publications

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“…After 30 days the only major degradants observed were gentamines arising from the cleavage of the A-ring from the B-C gentamicin ring system. All the LC–MS peaks observed in this study could be attributed to previously reported gentamicin impurities [30] , [31] , [32] . Thus, there was no evidence that gentamicin underwent substantive unique degradation pathways when applied as a device coating at readily detectable levels .…”

Section: Resultssupporting

confidence: 69%

“…The extracts obtained from the stability studies were also subjected to LC–MS analysis to screen for common gentamicin impurities and degradants. The characteristic ions for many of these gentamicin impurities have been previously reported [30] , [31] , [32] . Total ion count chromatograms showed the presence of the five gentamicin C components.…”

Section: Resultsmentioning

confidence: 79%

“…Bulk gentamicin mixtures as an active pharmaceutical ingredient (API) are typically characterized by high performance liquid chromatography (HPLC) with the detection of the major components facilitated by UV detection of their ortho -phthaldehyde derivatives [22] , [23] , pulsed electrochemical detection [24] , [25] , [26] , charged aerosol detection [27] or evaporative light scattering detection (ELSD) [24] , [28] , [29] . Liquid chromatography–mass spectrometry (LC–MS) has also been employed to establish impurity profiles of gentamicin mixtures [30] , [31] , [32] .

Fig.…”

Section: Introductionmentioning

confidence: 99%

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The impact of storage conditions upon gentamicin coated antimicrobial implants

Mullins

Deadman

Moynihan

et al. 2016

Journal of Pharmaceutical Analysis

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A systematic approach was developed to investigate the stability of gentamicin sulfate (GS) and GS/poly (lactic-co-glycolic acid) (PLGA) coatings on hydroxyapatite surfaces. The influence of environmental factors (light, humidity, oxidation and heat) upon degradation of the drug in the coatings was investigated using liquid chromatography with evaporative light scattering detection and mass spectrometry. GS coated rods were found to be stable across the range of environments assessed, with only an oxidizing atmosphere resulting in significant changes to the gentamicin composition. In contrast, rods coated with GS/PLGA were more sensitive to storage conditions with compositional changes being detected after storage at 60 °C, 75% relative humidity or exposure to light. The effect of γ-irradiation on the coated rods was also investigated and found to have no significant effect. Finally, liquid chromatography–mass spectrometry analysis revealed that known gentamines C1, C1a and C2 were the major degradants formed. Forced degradation of gentamicin coatings did not produce any unexpected degradants or impurities.

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Section: Resultssupporting

confidence: 69%

Section: Resultsmentioning

confidence: 79%

Fig.…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

The impact of storage conditions upon gentamicin coated antimicrobial implants

Mullins

Deadman

Moynihan

et al. 2016

Journal of Pharmaceutical Analysis

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“…LC equipped with ion trap MS with positive ionization was performed on a Capcell Pak C18 (AQ) column with the mobile phase containing 50 mM trifluoroacetic (TFA) and methanol for the determination of Gentamicin in bulk samples [122] .…”

Section: Chromatographic Methodsmentioning

confidence: 99%

Analytical methods for the determination of certain antibiotics used in critically ill patients

Ibrahim

El-Adl

Baraka

et al. 2020

J Pharm Biopharm Res

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Fast determination of underivatized gentamicin C components and impurities by LC-MS using a porous graphitic carbon stationary phase

et al. 2015

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Gentamicin C antibiotics are important because they are active against many multidrug-resistant Gram-negative bacilli. Unfortunately, their clinical usefulness is limited by their toxicity. Because of the difficulty involved in separating its different components, the US and European pharmacopeias both specify that the composition of gentamicin C should be determined by liquid chromatography with pulsed electrochemical detection. Here, we assess the usefulness of a porous graphitic carbon (PGC) HPLC column for separating the components of gentamicin C, and report chromatographic conditions that enable its direct characterization by PGC chromatography directly coupled to electrospray mass spectrometry. Native major components of gentamicin and impurities in commercial formulations were retained and separated on the PGC column without any need for derivatization, using mobile phases basified with ammonium hydroxide. When coupled with detection by conventional electrospray ion trap mass spectrometry (ESI-IT-MS), several previously reported impurities were detected easily, including the most polar gentamicin impurity, garamine. When operating in full-scan mode, it was possible to identify and quantitate gentamicin-related compounds using injected samples of only a few picograms. Under the described conditions, all analytes were eluted in less than 10 min and the LC-MS analyses exhibited excellent stability and linearity. The method's effectiveness was evaluated by analyzing commercial gentamicin batches and in-house formulations. When the PGC chromatographic system was coupled to an evaporative light-scattering detector, detection limits of 40-70 ng were achieved for various major gentamicin components. The chromatographic method was applied on a semi-preparative scale to purify the five major components.

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

Cited by 3 publications

References 41 publications

The impact of storage conditions upon gentamicin coated antimicrobial implants

The impact of storage conditions upon gentamicin coated antimicrobial implants

Analytical methods for the determination of certain antibiotics used in critically ill patients

Fast determination of underivatized gentamicin C components and impurities by LC-MS using a porous graphitic carbon stationary phase

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