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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 26, Number 6, September 2002,
pp. 313-319
Determination of Capsaicin, Nonivamide, and Dihydrocapsaicin
in Blood and Tissue by Liquid Chromatography–Tandem Mass Spectrometry
Christopher A. Reilly[1], Dennis J. Crouch[1], Garold S.
Yost[1], and Alim A. Fatah[2]
[1]Center for Human Toxicology and Department of Pharmacology and Toxicology,
University of Utah, Salt Lake City, Utah 84112
[2]Office of Law Enforcement Standards, National Institute of Standards and
Technology, 100 Bureau Drive, Stop #8102, Gaithersburg, Maryland 20899-8102
A sensitive and selective
liquid chromatography–tandem mass spectrometry (LC–MS–MS) method
for the analysis of capsaicin, nonivamide, and dihydrocapsaicin in blood and
tissue has been developed. The method utilized a one-step liquid–liquid
extraction that yielded an approximate 90% recovery of capsaicinoids from blood.
Chomatographic separation of the capsaicinoids was achieved using a reversed-phase
high-performance liquid chromatography column and a stepwise gradient of methanol
and distilled water containing 0.1% (v/v) formic acid. Identification and quantitation
of the capsaicinoids was achieved using electrospray ionization-tandem mass
spectrometry monitoring the precursor-to-product-ion transitions for the internal
standard octanoyl vanillamide (m/z 280 → 137), capsaicin (m/z 306 →
137), dihydrocapsaicin (m/z 308 → 137), and nonivamide (m/z 294 →
137). Calibration curves, 1.0 to 250 ng/mL, were constructed by plotting concentration
versus peak-area ratio (analyte/internal standard) and fitting the data with
a weighted quadratic equation. The accuracy of the assay ranged from 90% to
107% for all analytes. The intra-assay precision (%RSD) for capsaicin was 4%
at 2.5 ng/mL, 3% at 10 ng/mL, and 7% at 100 ng/mL. The interassay precision
(%RSD) for capsaicin was 6% at 2.5 ng/mL, 6% at 10 ng/mL, and 7% at 100 ng/mL.
Similar values for inter- and intra-assay precision were obtained for nonivamide
and dihydrocapsaicin. This method was used to assay for capsaicinoids in blood
and tissue samples collected from rats exposed to capsaicinoids via nose-only
inhalation. The concentration of capsaicin in these samples ranged from <
1.0 to 90.4 ng/mL in the blood, < 5.0 to 167 pg/mg in the lung, and <
2.0 to 3.4 pg/mg in the liver. Reproduction
of editorial content of this journal is prohibited without publisher’s
permission.
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