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Determination of cotinine in urine using glass capillary gas chromatography and selective detection, with special reference to the biological monitoring of passive smoking

Skarping, Gunnar LU ; Willers, Stefan LU and Dalene, Marianne LU (1988) In Journal of Chromatography A 454. p.293-301
Abstract
A capillary gas chromatographic (GC) method using selected-ion monitoring (SIM) was developed for the analysis of cotinine (C.A.S. No. 486-56-6) in human urine. The method is based on basic extraction of cotinine from 2 ml of urine into dichloromethane. After evaporation of the dichloromethane solution to dryness, 100 microliters of toluene were added, prior to GC-mass spectrometric (MS) analysis. Trideuterated cotinine (C.A.S. No. 97664-65-8) was used as the internal standard. More than 1000 automatic chromatographic analyses were made without column degradation. Molecular ions (M) of cotinine and trideuterated cotinine, (m/e = 176 and 179), were monitored in the electron impact (EI) mode and m/e = 177 (M + 1) and m/e = 180 (M + 1) in the... (More)
A capillary gas chromatographic (GC) method using selected-ion monitoring (SIM) was developed for the analysis of cotinine (C.A.S. No. 486-56-6) in human urine. The method is based on basic extraction of cotinine from 2 ml of urine into dichloromethane. After evaporation of the dichloromethane solution to dryness, 100 microliters of toluene were added, prior to GC-mass spectrometric (MS) analysis. Trideuterated cotinine (C.A.S. No. 97664-65-8) was used as the internal standard. More than 1000 automatic chromatographic analyses were made without column degradation. Molecular ions (M) of cotinine and trideuterated cotinine, (m/e = 176 and 179), were monitored in the electron impact (EI) mode and m/e = 177 (M + 1) and m/e = 180 (M + 1) in the chemical ionization (CI) mode with isobutane. The correlation coefficient with SIM and EI was 0.998 (5-20 ng/ml) and with CI was (0.2-2 ng/ml). For thermionic specific detection the correlation coefficient was 0.998 (10-510 ng/ml). Only capillary columns with an apolar bonded stationary phase film thickness of 1 micron showed sufficient inertness for cotinine analysis at the sub ng/ml level. The relative standard deviations for 5 and 20 ng/ml were 5.2 and 3.5% respectively (n = 12) using EI. Spiked urine samples from six non-smokers (5 ng/ml) showed a relative standard deviation of 5%. The overall recovery (25 ng/ml) was 100 +/- 4%. The minimum detectable concentration, using SIM, was ca. 2 ng/ml in the EI mode and ca. 0.2 ng/ml in the CI mode. The half-time for cotinine was ca. 18 h for both active smokers and non-smokers. (Less)
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author
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organization
publishing date
type
Contribution to journal
publication status
published
subject
in
Journal of Chromatography A
volume
454
pages
293 - 301
publisher
Elsevier
external identifiers
  • pmid:3235599
  • scopus:0023737921
ISSN
0021-9673
language
English
LU publication?
yes
id
a64a468c-25ba-444d-820b-289678bc6b9e (old id 1104331)
date added to LUP
2016-04-01 16:00:54
date last changed
2025-04-04 14:55:24
@article{a64a468c-25ba-444d-820b-289678bc6b9e,
  abstract     = {{A capillary gas chromatographic (GC) method using selected-ion monitoring (SIM) was developed for the analysis of cotinine (C.A.S. No. 486-56-6) in human urine. The method is based on basic extraction of cotinine from 2 ml of urine into dichloromethane. After evaporation of the dichloromethane solution to dryness, 100 microliters of toluene were added, prior to GC-mass spectrometric (MS) analysis. Trideuterated cotinine (C.A.S. No. 97664-65-8) was used as the internal standard. More than 1000 automatic chromatographic analyses were made without column degradation. Molecular ions (M) of cotinine and trideuterated cotinine, (m/e = 176 and 179), were monitored in the electron impact (EI) mode and m/e = 177 (M + 1) and m/e = 180 (M + 1) in the chemical ionization (CI) mode with isobutane. The correlation coefficient with SIM and EI was 0.998 (5-20 ng/ml) and with CI was (0.2-2 ng/ml). For thermionic specific detection the correlation coefficient was 0.998 (10-510 ng/ml). Only capillary columns with an apolar bonded stationary phase film thickness of 1 micron showed sufficient inertness for cotinine analysis at the sub ng/ml level. The relative standard deviations for 5 and 20 ng/ml were 5.2 and 3.5% respectively (n = 12) using EI. Spiked urine samples from six non-smokers (5 ng/ml) showed a relative standard deviation of 5%. The overall recovery (25 ng/ml) was 100 +/- 4%. The minimum detectable concentration, using SIM, was ca. 2 ng/ml in the EI mode and ca. 0.2 ng/ml in the CI mode. The half-time for cotinine was ca. 18 h for both active smokers and non-smokers.}},
  author       = {{Skarping, Gunnar and Willers, Stefan and Dalene, Marianne}},
  issn         = {{0021-9673}},
  language     = {{eng}},
  pages        = {{293--301}},
  publisher    = {{Elsevier}},
  series       = {{Journal of Chromatography A}},
  title        = {{Determination of cotinine in urine using glass capillary gas chromatography and selective detection, with special reference to the biological monitoring of passive smoking}},
  volume       = {{454}},
  year         = {{1988}},
}