Selective detection of carbon-13, nitrogen-15, and deuterium labeled metabolites by capillary gas chromatography-chemical reaction interface/mass spectrometry

Journal Article · Fri Dec 15 04:00:00 EST 1989 · Analytical Chemistry (Washington); (USA)

DOI:https://doi.org/10.1021/ac00199a009· OSTI ID:7026889

Chace, D H; Abramson, F P

We have applied a new chemical reaction interface/mass spectrometer technique (CRIMS) to the selective detection of 13C-, 15N-, and 2H-labeled phenytoin and its metabolites in urine following separation by capillary gas chromatography. The microwave-powered chemical reaction interface converts materials from their original forms into small molecules whose mass spectra serve to identify and quantify the nuclides that make up each analyte. The presence of each element is followed by monitoring the isotopic variants of CO2, NO, or H2 that are produced by the chemical reaction interface. Chromatograms showing only enriched 13C and 15N were produced by subtracting the abundance of naturally occurring isotopes from the observed M + 1 signal. A selective chromatogram of 2H (D) was obtained by measuring HD at m/z 3.0219 with a resolution of 2000. Metabolites representing less than 1.5% of the total labeled compounds could be identified in the chromatogram. Detection limits from urine of 380 pg/mL of a 15N-labeled metabolite, 7 ng/mL of a 13C-labeled metabolite, and 16 ng/mL of a deuterium labeled metabolite were determined at a signal to noise ratio of 2. Depending on the isotope examined, a linear dynamic range of 250-1000 was observed using CRIMS. To identify many of these labeled peaks (metabolites), the chromatographic analysis was repeated with the chemical reaction interface turned off and mass spectra obtained at the retention times found in the CRIMS experiment. CRIMS is a new analytical method that appears to be particularly useful for metabolism studies.

• OSTI ID: 7026889
• Journal Information: Analytical Chemistry (Washington); (USA), Journal Name: Analytical Chemistry (Washington); (USA) Vol. 61:24; ISSN 0003-2700; ISSN ANCHA
• Country of Publication: United States
• Language: English

Related Subjects

550501* -- Metabolism-- Tracer Techniques
59 BASIC BIOLOGICAL SCIENCES
ANIMALS
BIOLOGICAL MATERIALS
BIOLOGICAL WASTES
BODY FLUIDS
CARBON 13
CARBON ISOTOPES
CHROMATOGRAPHY
DEUTERIUM
DOGS
EVEN-ODD NUCLEI
GAS CHROMATOGRAPHY
HYDROGEN ISOTOPES
ISOTOPE APPLICATIONS
ISOTOPES
LABELLING
LIGHT NUCLEI
MAMMALS
MASS SPECTROSCOPY
MATERIALS
METABOLISM
METABOLITES
NITROGEN 15
NITROGEN ISOTOPES
NUCLEI
ODD-EVEN NUCLEI
ODD-ODD NUCLEI
ORGANIC COMPOUNDS
PROTEINS
SEPARATION PROCESSES
SIGNAL-TO-NOISE RATIO
SPECTROSCOPY
STABLE ISOTOPES
TRACER TECHNIQUES
URINE
VERTEBRATES
WASTES