A rapid simple pyrolysis derivatisation gas chromatography-mass spectrometry method for profiling of fatty acids in trace quantities of lipids

Challinor, J.M.

doi:10.1016/0165-2370(96)00946-1

Cited by 83 publications

(34 citation statements)

References 17 publications

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“…m-NBA was the matrix used for all the studies reported here. All fatty acids were purchased from Aldrich Chem Co. and esterified using MeOH or methanol-d 4 , using a standard esterification procedure. 24 The FAMEs studied are listed in Table 1.…”

Section: Experimental Parametersmentioning

confidence: 99%

“…picolinyl esters, 2a oxazolines, 2b labelled deutero diimide followed by pyrrolidides 2c or more commonly used dimethyl disulphide 2d derivatizations, etc., with a few exceptions which are fast and facile, e.g. microwave induced fast derivatizations 3 or in-situ derivatizations, 4 but which are not universal. Certain chemical ionization reagents were also used for double bond location, of which nitric oxide (NO) is important.…”

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confidence: 99%

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Liquid secondary ion mass spectral study of fatty acid methyl esters: silver cationization and collision induced dissociation studies

Kaveti

Raju

Vairamani

1997

Rapid Commun. Mass Spectrom.

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A preliminary investigation of silver ion interactions with saturated and unsaturated fatty acid methyl esters under liquid-assisted secondary ion mass spectral conditions is reported. Collision induced dissociation studies of silver cationized species, [M + Ag] + , have shown regular charge remote fragmentation, characteristic of cationized species, in addition to series of ions, due to addition of Ag + to the double bond in the case of the unsaturated compounds studied. These results are further substantiated by deuterium labelling.

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Section: Experimental Parametersmentioning

confidence: 99%

mentioning

confidence: 99%

Liquid secondary ion mass spectral study of fatty acid methyl esters: silver cationization and collision induced dissociation studies

Kaveti

Raju

Vairamani

1997

Rapid Commun. Mass Spectrom.

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“…C1s:2 and C1s:3 could not be detected if TMAH was used. Most likely this is caused by isomerisation and degradation reaction which is in consistence with data from the literature [4,6,12,16].…”

Section: S-286mentioning

confidence: 63%

“…Challinor was able to prevent isomerization by using (m-trifluoro-methyl-phenyl)-trimethylammonium hydroxide (MethPrepl) as methylation reagent. But the yield of fatty acid methyl esters (FAMEs) decreased [6]. Ishida et al used trimethylsulfonium hydroxide (TMSH) as reagent at a temperature of 350 ~ to suppress isomerization or degradation of FAMEs [13].…”

Section: Introductionmentioning

confidence: 99%

Studies of thermally assisted hydrolysis and methylation-GC-MS of fatty acids and triglycerides using different reagents and injection systems

2003

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SummaryThis work describes methodical studies of thermally assisted hydrolysis and methylation (THM) of fatty acids (FA) and triglycerides comparing different derivatization reagents, such as tetramethylammonium hydroxide (TMAH), tetramethylammonium acetate (TMAAc), trimethylsulfonium hydroxide (TMSH), trimethylphenylamine hydroxide (TMPAH), and (m-trifluoromethylphenyl) trimethylammonium hydroxide (MethPrep 2). The performance of these reagents using different injection techniques, such as pyrolysis, hot split injection, and programmed temperature vaporization (PTV) has been investigated.Itwas found that the PTV-injection can be used for quantitative in-situ methylation of free fatly acids. THM of triglycerides in a PTV injector is less effective than THM in a pyrolyzer. The highest yields of fatly acid methyl esters (FAMEs) were obtained using TMPAH as reagent. Generally THM of unsaturated triglycerides did not result in complete trans-methylation.

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“…Direct pyrolysis of glycerides, however, produces, among other products, fatty acids, which are not easily analysed by GC. The procedure introduced by Challinor [3], the so-called thermally assisted hydrolysis and methylation (THM), consisting of pyrolysis in combination with the methylating reagent TMAH (tetramethylammonium hydroxide), has been shown to be advantageous for the analysis of egg tempera and siccative oils [4][5][6]. Hydrolysis of ester groups promoted by TMAH in the heated pyrolysis chamber generates fatty acid salts which are subsequently methylated.…”

Section: Introductionmentioning

confidence: 99%

In-situ pyrolysis and silylation for analysis of lipid materials used in paint layers

2001

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SummaryAlthough pyrolysis coupled with gas chromatography and mass spectrometry (Py-GC-MS) is a useful technique for the rapid characterization of the organic materials used by artists, diagnostic pyrolysis products bearing polar groups, for example carboxylic acids, require derivatization (e.g. methylation) before GC separation. In this study we propose the use of hexamethyldisilazane (HMDS) as an effective on-line derivatizing reagent to prepare the trimethylsilyl (TMS) derivatives of fatty acids released from the pyrolysis of fats. Pyrolysis in combination with HMDS has been applied to the analysis of lipid materials employed as painting media, for example siccative oils and egg.

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A rapid simple pyrolysis derivatisation gas chromatography-mass spectrometry method for profiling of fatty acids in trace quantities of lipids

Cited by 83 publications

References 17 publications

Liquid secondary ion mass spectral study of fatty acid methyl esters: silver cationization and collision induced dissociation studies

Liquid secondary ion mass spectral study of fatty acid methyl esters: silver cationization and collision induced dissociation studies

Studies of thermally assisted hydrolysis and methylation-GC-MS of fatty acids and triglycerides using different reagents and injection systems

In-situ pyrolysis and silylation for analysis of lipid materials used in paint layers

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