Silylation of carbonyl compounds in a chromato-mass spectrometer column

Yatsenko, A. E.; Mikaya, A. I.; Glebov, L. S.; Заикин, В. Г.

doi:10.1007/bf00953259

Cited by 2 publications

(2 citation statements)

References 3 publications

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“…The reaction can proceed within the GC column and enable mass spectra of enol-ethers obtained from aldehydes and ketones to be recorded. 48 On-column formation of imines was observed in the study of carbonyl compounds by NH 3 chemical ionization GC/MS. Respective imines were also formed by the injection of an amine immediately after the introduction of a carbonyl compound.…”

Section: On-column �Erivatizationmentioning

confidence: 99%

Derivatization in Mass Spectrometry—7. On-Line Derivatization/Degradation

Halket

Заикин

2006

Eur J Mass Spectrom (Chichester)

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The review describes on-line derivatization/degradation methods employed in mass spectrometry to solve some structural and analytical problems. Advantages and applications of various positions of reaction systems connected mainly to a mass spectrometer or a gas chromatograph/mass spectrometer are considered. Among these are reaction systems connected directly to the mass spectrometer (reaction mass spectrometry, pyrolysis-mass spectrometry or direct pyrolysis-mass spectrometry); flash-heaters as reactors in gas chromatography/mass spectrometry (GC/MS); in-line chemical reactors located before the chromatographic column [pre-column derivatization/degradation with the use of catalytic reactions, pyrolysis (pyrolysis-GC/MS), degradation in elemental analyzers-isotope ratio mass pectrometry (EA-IRMS)]; on-column derivatization and deuteration; reactor located between the chromatographic column and a mass spectrometer [post-column catalytic derivatization, gas chromatograph-combustion-isotope ratio mass spectrometer (GC-c-IRMS)]. Post-column derivatization in high performance liquid chromatography/mass spectro-metry is briefly mentioned. Application of such on-line methodology to structure elucidation of low molecular mass compounds and polymers, to the determination of isotope ratios of the most common elements, to the investigation of catalytic reactions is discussed..

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Section: On-column �Erivatizationmentioning

confidence: 99%

Derivatization in Mass Spectrometry—7. On-Line Derivatization/Degradation

Halket

Заикин

2006

Eur J Mass Spectrom (Chichester)

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“…Such derivatives can also be obtained by on-column silylation by successive admission of carbonyl compounds and silylating agents (BSTFA + 1% Me 3 SiCl) into the flash heater of a gas chromatograph. 157 It was mentioned that the greater the amount of silylating reagent used, the greater the yield of enol silyl ethers obtained. One should keep in mind that only one product is formed in the case of aldehydes, whereas the silylation of ketones usually give rise to a mixture of isomeric enol silyl ethers: The abundant peak at m/z 127 in the spectrum of the TMS ether prepared from cyclohexanone may be formed as follows:…”

Section: Derivatization Of Aldehydes and Ketonesmentioning

confidence: 99%

Derivatization in Mass Spectrometry—5. Specific Derivatization of Monofunctional Compounds

Halket

Заикин

2005

Eur J Mass Spectrom (Chichester)

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The present paper is complementary to the foregoing reviews and describes some additional methods of the derivatization of particular functional groups mainly to enhance the structural information content of electron ionization and chemical ionization mass spectra. Derivatization approaches for the modification of unsaturated compounds, alcoholic, carboxylic, carbonyl, amine and other functional groups, are discussed. Derivatization for separation and quantitative determination of chiral enantiomeric compounds is also considered. Preliminary chemical and physical-chemical degradation for structure elucidation of high molecular weight compounds (biopolymers, synthetic polymers) is mentioned. Chemical aspects of derivatizations and characteristic mass spectral features of derivatives are described briefly. Some particular applications of chemical modification, in conjunction with mass spectral measurements for the analysis of various important bioorganic compounds and compounds in biological fluids, air, environmental etc., are considered.

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Silylation of carbonyl compounds in a chromato-mass spectrometer column

Cited by 2 publications

References 3 publications

Derivatization in Mass Spectrometry—7. On-Line Derivatization/Degradation

Derivatization in Mass Spectrometry—7. On-Line Derivatization/Degradation

Derivatization in Mass Spectrometry—5. Specific Derivatization of Monofunctional Compounds

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