Analysis of thyroid hormones as their heptafluorobutyryl methyl ester derivatives by gas chromatography - mass spectrometry

Petersen, B.A.; Vouros, Paul

doi:10.1021/ac50017a006

Cited by 16 publications

(3 citation statements)

References 26 publications

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“…For GC, the N,O-di-HFB methyl ester derivatives were formed. The EI mass spectra (shown in Figs 1 and 2) match those previously published by Petersen et al 8 Note that the respective molecular ions at m/z 1057 and 1066 were beyond the mass range of our instrument. The abundant ions at m/z 844 and 853 were selected for quantification of T3/ 13 C 9 -T3 using SIM.…”

Section: Resultssupporting

confidence: 85%

“…The abundant ions at m/z 844 and 853 were selected for quantification of T3/ 13 C 9 -T3 using SIM. These fragment ions correspond to [M À C 3 F 7 CONH 2 ] Á , formed via a McLafferty rearrangement, as described in detail in Ref 8 . Figure 3 shows the mass spectra obtained for T3 and 13 C 9 -T3 using LC/ESI-MS in positive ion mode.…”

Section: Resultsmentioning

confidence: 98%

“…[4][5][6] For T4, several ID-MS reference methods combined with gas chromatography (ID-GC/MS) 6 or electrospray ionization liquid chromatography (ESI ID-LC/MS) 7 have been developed. Analysis of T3 by GC/MS was, to the best of our knowledge, restricted to standards for studying the characteristics of volatile derivatives, 8,9 without reference to applications of serum analysis. This was mainly due to the much lower concentration of T3 in serum ($1 ng/mL) compared with T4 ($100 ng/mL).…”

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confidence: 99%

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Isotope dilution-gas chromatography/mass spectrometry and liquid chromatography/electrospray ionization-tandem mass spectrometry for the determination of triiodo-L-thyronine in serum

Thienpont

Fierens

Leenheer

et al. 1999

Rapid Commun. Mass Spectrom.

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Isotope dilution-gas chromatography/mass spectrometry (ID-GC/MS) and isotope dilution-liquid chromatography/tandem mass spectrometry (ID-LC/MS/MS) methods have been developed for an determination of triiodothyronine (T3) in serum and their potential as candidate reference methods investigated. In both methods, (13)C(9)-T3 was used as internal standard. Sample pretreatment consisted of deproteinization, extraction and high performance liquid chromatography (HPLC) purification. Conversion of serum thyroxine (T4) to T3 was controlled by adding (13)C(6)-T4. For GC/MS, T3 and (13)C(9)-T3 were converted to the N,O-di-heptafluorobutyryl (HFB) methyl ester derivatives and monitored at m/z 844 and 853. For LC/MS with electrospray ionization, the transitions m/z 652/661 to 606/614 were monitored. For use of the methods as candidate reference methods, special attention was paid to the calibration and the measurement protocol (duplicate analysis of each sample on three occasions). Evaluation of the ID-GC/MS and ID-LC/MS/MS methods showed the absence of interference by reverse T3 and T4, a limit of detection of 100 pg (GC/MS) and 18 pg (LC/MS), a recovery of 100 +/- 1.5% (95% confidence interval) and good precision (the total coefficient of variation, n = 6, was typically 1.5%). In addition to the recovery study, the accuracy of the methods was proven by method comparison (ID-GC/MS vs. LC/MS/MS) on three sera, showing a maximum deviation of 1.1%. Finally, the ID-GC/MS method was applied for measurement of 10 different human sera with a T3 concentration range from 0.6 to 7.3 ng/mL.

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Section: Resultssupporting

confidence: 85%

Section: Resultsmentioning

confidence: 98%

mentioning

confidence: 99%

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Isotope dilution-gas chromatography/mass spectrometry and liquid chromatography/electrospray ionization-tandem mass spectrometry for the determination of triiodo-L-thyronine in serum

Thienpont

Fierens

Leenheer

et al. 1999

Rapid Commun. Mass Spectrom.

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Some considerations on quantitative methodology and detection limits in organic mass spectrometry

Marshall¹,

Petersen

Vouros

1978

Biol. Mass Spectrom.

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Mass spectrometric sensitivity data for the compounds cholesterol, cholestane, DDT, decafluorotriphenylphosphine, morphine, LSD and methyl stearate have been developed over a period of time and under a variety of conditions. This information is presented on both a relative and an absolute basis. With the exception of morphine, relative sensitivies were reproducible to within a factor of three over a six month period. This reproducibility facilitates quantitation and a single standard can be used for calibration of organic compounds from various classes. Detection limits of 50 femtograms for LSD are realized for samples introduced via the direct inlet probe.

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3,5-diiodotyrosine excretion in human urine in individuals of differing thyroidal status

Mohammed

Farmer

Ramsden

1983

Biol. Mass Spectrom.

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The urinary excretion of 3,5-diiodotyrosine was determined in euthyroid, hypothyroid and hyperthyroid individuals using a sensitive gas chromatographic mass spectrometric assay. This involved a multi-step extraction of the amino acid from urine (mean efficiency 28 +/- 5.7%) then conversion to the N,O-diheptafluorobutyryl methyl ester. The fragmentation of the derivative is discussed. Although the mean excretions in the two pathological states were significantly different from that of euthyroid individuals (P less than 0.01 in both instances) there was considerable overlap with the normal range.

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Analysis of thyroid hormones as their heptafluorobutyryl methyl ester derivatives by gas chromatography - mass spectrometry

Cited by 16 publications

References 26 publications

Isotope dilution-gas chromatography/mass spectrometry and liquid chromatography/electrospray ionization-tandem mass spectrometry for the determination of triiodo-L-thyronine in serum

Isotope dilution-gas chromatography/mass spectrometry and liquid chromatography/electrospray ionization-tandem mass spectrometry for the determination of triiodo-L-thyronine in serum

Some considerations on quantitative methodology and detection limits in organic mass spectrometry

3,5-diiodotyrosine excretion in human urine in individuals of differing thyroidal status

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