Determination of very-long-chain fatty acids in serum by gas chromatography–nitrogen–phosphorus detection following cyanomethylation

Paik, Man‐Jeong; KyungOk, Lee; Shin, Ho‐Sang

doi:10.1016/s0378-4347(98)00436-8

Cited by 17 publications

(5 citation statements)

References 17 publications

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“…78 Bromoacetonitrile was suggested as an alkylating reagent to improve the nitrogen-phosphorous detection of very long-chain fatty acids in GC. 79 EI mass spectra of the derivatives of straight-chain acids presented in the paper reveal rather intense peaks for [M -C n H 2n+1 ] + ions (n ³ 1). It may be supposed that such derivatives can be used for the location of double bonds or branching points in other aliphatic acids.…”

Section: Some Mass Spectral Features Of Alkyl (Aryl) Derivativesmentioning

confidence: 77%

Derivatization in Mass Spectrometry– 3. Alkylation (Arylation)

Halket

Заикин

2004

Eur J Mass Spectrom (Chichester)

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The review is devoted to alkylation (arylation) as a widely employed derivatization procedure for the protection of OH (carboxylic acids, phosphoric acids, sulfonic acids, alcohols, polyols, phenols, enols), SH (thiols) and NH (amines, amides) groups in order to increase volatility, to improve the chromatographic properties and, if possible, mass spectral properties of derivatives. Chemical aspects of derivatization and various alkylation (arylation) reagents and reaction procedures are described. Specific mass spectral (electron ionization, chemical ionization) features of derivatives helpful in identification, structure elucidation, profiling and quantitative determination of the above-mentioned polar compounds by coupled gas chromatography or high-performance liquid chromatography are discussed. Some common analytical applications of the procedures in organic chemistry, clinical chemistry, environmental chemistry etc. are briefly summarized.

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Section: Some Mass Spectral Features Of Alkyl (Aryl) Derivativesmentioning

confidence: 77%

Derivatization in Mass Spectrometry– 3. Alkylation (Arylation)

Halket

Заикин

2004

Eur J Mass Spectrom (Chichester)

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“…The method validation was based on previous studies measuring endogenous fatty acids (Mauriala et al ., 2004; Paik et al ., 1999; Valianpour et al ., 2003; Chung et al ., 2008) while encompassing the expected concentration range in plasma before and after fish oil supplementation. Linearity and quantification limits for all analytes were evaluated by the analysis of calibration samples (0.5, 1.0, 5.0, 10, 25, 50, 100, 150, 200 and 300 mg/L) prepared in acetonitrile–water (75:25 v/v) and extracted as per the sample preparation procedure previously stated.…”

Section: Methodsmentioning

confidence: 99%

Simultaneous quantification of total eicosapentaenoic acid, docosahexaenoic acid and arachidonic acid in plasma by high‐performance liquid chromatography–tandem mass spectrometry

Salm

Taylor

Kostner³

2010

Biomedical Chromatography

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A method for the simultaneous quantification of eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA) and arachidonic acid (AA) in human plasma by HPLC-tandem mass spectrometry (HPLC-MS/MS) was developed and validated. Free and esterified forms of fatty acids were hydrolysed from plasma samples in the presence of an internal standard and subjected to liquid-liquid extraction. The chromatographic run time was 3.5 min per sample. The assay was linear from 0.5 to 300 mg/L (r(2) > 0.997, n = 18). Based on matrix addition, accuracy deviation was <15%, except for AA at 10 mg/L (30-90%), whereas precision was <8% for all fatty acids studied. The method was applied to the measurement of these omega-3 fatty acids in a fish oil supplement study with healthy volunteers. Healthy males (n = 4) were administered a supplement containing 465 mg EPA and 375 mg DHA per capsule (Omacor®). A dose of two capsules was given daily over a 4 week period. Pre-treatment concentrations varied between subjects for EPA (17-68 mg/L), DHA (36-63 mg/L) and AA (121-248 mg/L). During the dosing period EPA increased 460-480% from the baseline concentration, while DHA increased 150-160%. The EPA-AA ratio increased from 0.07-0.56 to 0.3-3.1 after 4 weeks of dosing. In conclusion, the method described could be suitable for monitoring EPA, DHA and AA in clinical studies that may aid in achieving optimal concentrations of these fatty acids in patients who could be at risk of sudden cardiac death.

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“…Conventional analysis of biologically important fatty acids involves hydrolysis of lipid species to free fatty acids and conversion to methyl esters for gas chromatography (GC) 1,2 and gas chromatography/mass spectrometry (GC/MS) 3 or to aromatic esters for high pressure liquid chromatography with ultraviolet 4 or mass spectrometric detection. An additional purification step such as thin layer chromatography is sometimes required.…”

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confidence: 99%

Dimethylaminoethyl esters for trace, rapid analysis of fatty acids by electrospray tandem mass spectrometry

Johnson

1999

Rapid Commun. Mass Spectrom.

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The development of a new derivative, the dimethylaminoethyl ester, for the analysis of fatty acids by electrospray tandem mass spectrometry is described. Qualitative and quantitative analyses of long to very long chain fatty acids in plasma, blood, urine and wax were performed. Branched chain, unsaturated, dicarboxylic, hydroxy, amino and keto acids were studied. The quantitative analysis method using the new derivative is simple, rapid and precise with small sample size. It has good potential as a screening method for biologically important fatty acids. Copyright 1999 John Wiley & Sons, Ltd.

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Determination of very-long-chain fatty acids in serum by gas chromatography–nitrogen–phosphorus detection following cyanomethylation

Cited by 17 publications

References 17 publications

Derivatization in Mass Spectrometry– 3. Alkylation (Arylation)

Derivatization in Mass Spectrometry– 3. Alkylation (Arylation)

Simultaneous quantification of total eicosapentaenoic acid, docosahexaenoic acid and arachidonic acid in plasma by high‐performance liquid chromatography–tandem mass spectrometry

Dimethylaminoethyl esters for trace, rapid analysis of fatty acids by electrospray tandem mass spectrometry

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