Home  About us  Contact
 

Isotope Dilution Mass Spectrometry (isotope + dilution_mass_spectrometry)

Distribution by Scientific Domains
Chemistry100%

Selected Abstracts

Linearization of second-order calibration curves in stable isotope dilution,mass spectrometry

FLAVOUR AND FRAGRANCE JOURNAL, Issue 3 2001
Laurent B. Fay
Abstract The quantification of compounds using isotope dilution mass spectrometry requires the establishment of calibration curves prior to determination of any unknown sample. When calibration over a wide concentration range is required and/or when an overlap exists between internal standard and analyte ions (if mono- or di-isotopically-labelled internal standards are used), second-order calibration curves are obtained. In this paper we have compared several calculation methods to linearize such calibration curves. We found that the method published by Bush and Trager6 gives a satisfactory linear relationship between the corrected amount ratio y = Ql(Qu+tQl) (the value Qu being the amount of unlabelled analyte, Ql the amount of labelled internal standard and t, the fixed fraction of the internal standard, which is identical to the unlabelled analyte) and the ratio of unlabelled to labelled ion intensities. All the other calculation methods that have been published so far have failed to linearize the second-order calibration curve build-up over a wide concentration range. Copyright © 2001 John Wiley & Sons, Ltd. [source]

First results of a quantitative study of DNA adducts of melphalan in the rat by isotope dilution mass spectrometry using capillary liquid chromatography coupled to electrospray tandem mass spectrometry

RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 14 2005
Bart Van den Driessche
Rats were intravenously injected with a single high dose (10,mg/kg) of the alkylating agent melphalan in order to study DNA-adduct formation. Quantitation of a dGuo-melphalan adduct was done by isotope dilution mass spectrometry using capillary liquid chromatography/mass spectrometry (LC/MS) and [15N5]-labeled dGuo-melphalan as internal standard. DNA-adduct levels were studied in bone marrow, liver and kidney. The instrumental detection limit of the method was determined to be 900,fg (S/N 3, pure standard). These first results clearly show a 10 times higher adduct level in bone marrow compared to kidney and a 6 times higher level compared to liver. More experiments will be necessary to gather more information on the pharmacokinetics of melphalan-DNA adducts under in vivo conditions. Copyright © 2005 John Wiley & Sons, Ltd. [source]

Comparison of gas chromatography and liquid chromatography mass spectrometric measurements for high accuracy analysis of cholesterol in human serum by isotope dilution mass spectrometry

RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 9 2002
Céline S. J. Wolff Briche
Cholesterol measurements are of vital clinical importance and reliable reference materials are essential for method validation. Gas chromatography with mass spectrometry (GC/MS) is usually used for the high accuracy analysis of cholesterol by isotope dilution. A certified reference material for cholesterol content in human serum was analysed by isotope dilution utilising GC/MS and liquid chromatography mass spectrometry (LC/MS). The use of LC/MS avoided the need for a derivatisation step. Both LC/MS and GC/MS produced results on the measurement of cholesterol that agreed within 0.5% of the certified value. Moreover, the precision obtained for ratio measurement using both techniques are comparable and lead to relative expanded standard uncertainties (with a coverage factor of 2) varying between 0.2 and 0.5%. Copyright © 2002 John Wiley & Sons, Ltd. [source]

A novel approach for identification and measurement of hemoglobin adducts with 1,2,3,4-diepoxybutane by liquid chromatography/electrospray ionisation mass spectrometry and matrix-assisted laser desorption/ionisation tandem mass spectrometry

RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 8 2001
Adriana Basile
The structural characterisation of the adducts formed by in vitro interaction of hemoglobin (Hb) with 1,2,3,4-diepoxybutane (DEB), the most reactive 1,3-butadiene (BD) metabolite, was obtained by liquid chromatography/electrospray ionisation mass spectrometry (LC/ES-MS) analysis of modified tryptic peptides of human hemoglobin chains. The reactive sites of human hemoglobin towards DEB and its hydroxylated derivatives (trihydroxybutyl (THB)-derivatives) were identified through the characterisation of alkylated tryptic peptides by matrix-assisted laser desorption/ionisation tandem mass spectrometry (MALDI-MS/MS). Based on this characterisation, a procedure was set up to measure the Hb-adducts of THB-derivatives by isotope dilution mass spectrometry with the use of a deuterated peptide standard. The results obtained here could permit optimisation of molecular dosimetry of BD-adducts, and extension of the analysis to the biological monitoring of occupational exposure to butadiene. Copyright © 2001 John Wiley & Sons, Ltd. [source]