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采用毛细管液相色谱-电喷雾串联质谱法分析[3',3'-d(2)]-尼古丁和[3',3'-d(2)]-可替宁

Analysis of [3',3'-d(2)]-nicotine and [3',3'-d(2)]-cotinine by capillary liquid chromatography-electrospray tandem mass spectrometry.

作者信息

Murphy Sharon E, Villalta Peter, Ho Sing-Wei, von Weymarn Linda B

机构信息

University of Minnesota Cancer Center, Minneapolis, MN 55455, USA.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Sep 15;857(1):1-8. doi: 10.1016/j.jchromb.2007.06.018. Epub 2007 Jun 29.

DOI:10.1016/j.jchromb.2007.06.018
PMID:17644451
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC2234036/
Abstract

A selective and sensitive LC/MS/MS assay was developed for the quantification of d(2)-nicotine and d(2)-cotinine in plasma of current and past smokers administered d(2)-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 d(2)-nicotine (0.03-6.0 ng/ml plasma) and d(2)-cotinine (0.15-25 ng/ml plasma). The lower limits of quantitation were 0.15 ng/ml and 0.25 ng/ml for d(2)-nicotine and d(2)-cotinine, respectively. The coefficient of variation was 3.7% for d(2)-nicotine and 2.5% for d(2)-cotinine. The method was applied to two ongoing studies of d(2)-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.

摘要

建立了一种选择性和灵敏的液相色谱/串联质谱法,用于定量测定服用d(2)-尼古丁的现吸烟者和既往吸烟者血浆中的d(2)-尼古丁和d(2)-可替宁。经过固相萃取和液液萃取后,在毛细管亲水相互作用色谱柱上实现了高效液相色谱分离。通过电喷雾正离子化串联质谱法监测分析物。生成了d(2)-尼古丁(0.03-6.0 ng/ml血浆)和d(2)-可替宁(0.15-25 ng/ml血浆)的线性校准曲线。d(2)-尼古丁和d(2)-可替宁的定量下限分别为0.15 ng/ml和0.25 ng/ml。d(2)-尼古丁的变异系数为3.7%,d(2)-可替宁的变异系数为2.5%。该方法应用于两项关于既往吸烟者和现吸烟者d(2)-尼古丁代谢的正在进行的研究。对这些研究中一部分受试者的初步分析发现,与现吸烟者相比,既往吸烟者将尼古丁转化为可替宁的速率显著降低。

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