Analysis of amine compounds by capillary gas chromatography using ammonia–helium carrier gas

Ghaoui, L.; Pell, Karen; Chritz, Karen; Loomis, Robert N.

doi:10.1002/jhrc.1240180304

Cited by 9 publications

(2 citation statements)

References 8 publications

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“…4a even without the introduction of the sample. It should be noted that the finding of this deactivation effect is not novel, as it had long been exploited in GC using ammonia carrier gas for reducing the sample retention 25–27. However, it is fruitful for the optimization of the present ion source for the detection of high‐polar analytes such as amines.…”

Section: Resultsmentioning

confidence: 99%

Development of ambient sampling chemi/chemical ion source with dielectric barrier discharge

Chen

Furuya

et al. 2010

J. Mass Spectrom.

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The development of a new configuration of chemical ionization (CI)-based ion source is presented. The ambient air containing the gaseous sample is sniffed into an enclosed ionization chamber which is of sub-ambient pressure, and is subsequently mixed with metastable species in front of the ion inlet of the mass spectrometer. Metastable helium atoms (He*) are used in this study as the primary ionizing agents and are generated from a dielectric barrier discharge (DBD) source. The DBD is powered by an AC high-voltage supply and the configuration of the electrodes is in such a way that the generated plasma is confined within the discharge tube and is not extended into the ionization chamber. The construction of the ion source is simple, and volatile compounds released from the bulky sample can also be analyzed directly by approaching the sample to the sampling nozzle. When combined with heated nitrogen or other desorption methods, its application can also be extended to non-volatile compounds, and the consumption for helium can be kept minimum solely for maintaining the stable discharge and gas phase ionization. Applications to non-proximate sample analysis, direct determination of active ingredients in drug tablets and the detection of trace explosive such as hexamethylene triperoxide diamine are demonstrated.

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Section: Resultsmentioning

confidence: 99%

Development of ambient sampling chemi/chemical ion source with dielectric barrier discharge

Chen

Furuya

et al. 2010

J. Mass Spectrom.

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“…To overcome this, the column may be deactivated 8 or a specific column for amine analysis can be used. 9 Alternatively, ammonia has been added to the carrier gas, 10 but more often derivatisation is used; Kataoka has reviewed the derivatisation reactions used for the GC analysis of amines. 11,12 Capillary electrophoresis has been used for the analysis of amines but the sensitivity decreased with increasing molecular weight of the amines.…”

Section: Introductionmentioning

confidence: 99%

Towards a generic method for ion chromatography/mass spectrometry of low‐molecular‐weight amines in pharmaceutical drug discovery and development

Lewis

Jackson

Crampton

et al. 2020

Rapid Comm Mass Spectrometry

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Rationale Low‐molecular‐weight amines are encountered in pharmaceutical analysis, e.g. as reactants in chemical syntheses, but are challenging to analyse using ultrahigh‐performance liquid chromatography/mass spectrometry (UHPLC/MS) due to their high polarity causing poor retention. Ion chromatography/mass spectrometry (IC/MS) is an emerging technique for polar molecule analysis that offers better separation. A generic IC/MS method would overcome problems associated with using UHPLC/MS in drug discovery and development environments. Methods Amine standards were analysed using IC/MS with gradient elution (variety of column temperatures evaluated). An electrospray ionisation (ESI) quadrupole mass spectrometer was operated in positive ion polarity in scanning mode. The make‐up flow composition was evaluated by assessing the performance of a range of organic modifiers (acetonitrile, ethanol, methanol) and additives (acetic acid, formic acid, methanesulfonic acid). The ESI conditions were optimised to minimise adduct formation and promote generation of protonated molecules. Results The performance attributes were investigated and optimised for low‐molecular‐weight amine analysis. Organic solvents and acidic additives were evaluated as make‐up flow components to promote ESI, with 0.05% acetic acid in ethanol optimal for producing protonated molecules. The hydrogen bonding capability of amines led to abundant protonated molecule–solvent complexes; optimisation of source conditions reduced these, with collision‐induced dissociation voltage having a strong effect. The detection limit was ≤1.78 ng for the amines analysed, which is fit‐for‐purpose for an open‐access chemistry environment. Conclusions This study demonstrates the value of IC/MS for analysing low‐molecular‐weight amines. Good chromatographic separation of mixtures was possible without derivatisation. Ionisation efficiency was greatest using a make‐up flow of 0.05% acetic acid in ethanol, and optimisation of ESI source conditions promoted protonated molecule generation for easy determination of molecular weight.

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Review of interactive carrier gases including ammonia in gas liquid chromatography

Abdel‐Rehim

1999

J. Micro. Sep.

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Analysis of amine compounds by capillary gas chromatography using ammonia–helium carrier gas

Cited by 9 publications

References 8 publications

Development of ambient sampling chemi/chemical ion source with dielectric barrier discharge

Development of ambient sampling chemi/chemical ion source with dielectric barrier discharge

Towards a generic method for ion chromatography/mass spectrometry of low‐molecular‐weight amines in pharmaceutical drug discovery and development

Review of interactive carrier gases including ammonia in gas liquid chromatography

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