Analysis of [3′,3′-d2]-nicotine and [3′,3′-d2]-cotinine by capillary liquid chromatography-electrospray tandem mass spectrometry

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Abstract

A selective and sensitive LC/MS/MS assay was developed for the quantification of d2-nicotine and d2-cotinine in plasma of current and past smokers administered d2-nicotine. After solid phase extraction and liquid-liquid extraction, HPLC separation was achieved on a capillary hydrophilic interaction chromatography phase column. The analytes were monitored by tandem mass spectrometry with electrospray positive ionization. Linear calibration curves were generated for d2-nicotine (0.03-6.0 ng/ml plasma) and d2-cotinine (0.15-25 ng/ml plasma). The lower limits of quantitation were 0.15 ng/ml and 0.25 ng/ml for d2-nicotine and d2-cotinine, respectively. The coefficient of variation was 3.7% for d2-nicotine and 2.5% for d2-cotinine. The method was applied to two ongoing studies of d2-nicotine metabolism in prior and current smokers. Preliminary analysis of a subset of subjects from these studies detected a significantly lower rate of nicotine conversion to cotinine by past smokers compared to current smokers.

Original languageEnglish (US)
Pages (from-to)1-8
Number of pages8
JournalJournal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
Volume857
Issue number1
DOIs
StatePublished - Sep 15 2007

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Cotinine
Liquid chromatography
Tandem Mass Spectrometry
Nicotine
Liquid Chromatography
Mass spectrometry
Plasmas
Liquid-Liquid Extraction
Solid Phase Extraction
Liquids
Chromatography
Hydrophobic and Hydrophilic Interactions
Metabolism
Calibration
Ionization
Assays
High Pressure Liquid Chromatography

Keywords

  • HILIC
  • Nicotine metabolism
  • d2-nicotine

Cite this

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title = "Analysis of [3′,3′-d2]-nicotine and [3′,3′-d2]-cotinine by capillary liquid chromatography-electrospray tandem mass spectrometry",
abstract = "A selective and sensitive LC/MS/MS assay was developed for the quantification of d2-nicotine and d2-cotinine in plasma of current and past smokers administered d2-nicotine. After solid phase extraction and liquid-liquid extraction, HPLC separation was achieved on a capillary hydrophilic interaction chromatography phase column. The analytes were monitored by tandem mass spectrometry with electrospray positive ionization. Linear calibration curves were generated for d2-nicotine (0.03-6.0 ng/ml plasma) and d2-cotinine (0.15-25 ng/ml plasma). The lower limits of quantitation were 0.15 ng/ml and 0.25 ng/ml for d2-nicotine and d2-cotinine, respectively. The coefficient of variation was 3.7{\%} for d2-nicotine and 2.5{\%} for d2-cotinine. The method was applied to two ongoing studies of d2-nicotine metabolism in prior and current smokers. Preliminary analysis of a subset of subjects from these studies detected a significantly lower rate of nicotine conversion to cotinine by past smokers compared to current smokers.",
keywords = "HILIC, Nicotine metabolism, d2-nicotine",
author = "Murphy, {Sharon E} and Villalta, {Peter W} and Ho, {Sing Wei} and {von Weymarn}, {Linda B}",
year = "2007",
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AU - Villalta, Peter W

AU - Ho, Sing Wei

AU - von Weymarn, Linda B

PY - 2007/9/15

Y1 - 2007/9/15

N2 - A selective and sensitive LC/MS/MS assay was developed for the quantification of d2-nicotine and d2-cotinine in plasma of current and past smokers administered d2-nicotine. After solid phase extraction and liquid-liquid extraction, HPLC separation was achieved on a capillary hydrophilic interaction chromatography phase column. The analytes were monitored by tandem mass spectrometry with electrospray positive ionization. Linear calibration curves were generated for d2-nicotine (0.03-6.0 ng/ml plasma) and d2-cotinine (0.15-25 ng/ml plasma). The lower limits of quantitation were 0.15 ng/ml and 0.25 ng/ml for d2-nicotine and d2-cotinine, respectively. The coefficient of variation was 3.7% for d2-nicotine and 2.5% for d2-cotinine. The method was applied to two ongoing studies of d2-nicotine metabolism in prior and current smokers. Preliminary analysis of a subset of subjects from these studies detected a significantly lower rate of nicotine conversion to cotinine by past smokers compared to current smokers.

AB - A selective and sensitive LC/MS/MS assay was developed for the quantification of d2-nicotine and d2-cotinine in plasma of current and past smokers administered d2-nicotine. After solid phase extraction and liquid-liquid extraction, HPLC separation was achieved on a capillary hydrophilic interaction chromatography phase column. The analytes were monitored by tandem mass spectrometry with electrospray positive ionization. Linear calibration curves were generated for d2-nicotine (0.03-6.0 ng/ml plasma) and d2-cotinine (0.15-25 ng/ml plasma). The lower limits of quantitation were 0.15 ng/ml and 0.25 ng/ml for d2-nicotine and d2-cotinine, respectively. The coefficient of variation was 3.7% for d2-nicotine and 2.5% for d2-cotinine. The method was applied to two ongoing studies of d2-nicotine metabolism in prior and current smokers. Preliminary analysis of a subset of subjects from these studies detected a significantly lower rate of nicotine conversion to cotinine by past smokers compared to current smokers.

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