Quantitation of Nicotine, Its Metabolites, and Other Related Alkaloids in Urine, Serum, and Plasma Using LC-MS-MS

Abstract

We describe a method for the quantitative analysis of nicotine, cotinine, trans-3'-hydroxy cotinine, nornicotine, and anabasine in urine, serum, and plasma using liquid chromatography-tandem mass spectrometry. A mix of deuterium-labeled internal standards (IS) is added to a specimen aliquot. The aliquot is extracted using mixed-mode solid phase extraction and eluted into an autosampler vial for injection into an LC-MS-MS system. An Atlantis silica column is used for LC separation in hydrophilic interaction mode. Tandem mass spectrometry detection is performed in positive ion mode with electrospray ionization and two multiple reaction monitoring (MRM) transitions monitored for each analyte and IS.

Quantification of nicotine, cotinine, trans-3′-hydroxycotinine and varenicline in human plasma by a sensitive and specific UPLC–tandem mass-spectrometry procedure for a clinical study on smoking cessation

“…Sample preparation was mostly performed by solid phase extraction (SPE) [8][9][10]12,15,16] or by liquid-liquid extraction (LLE) [13,19]. Several methods have been recently published for the quantification of nicotine and metabolites using hydrophilic interaction liquid chromatography (HILIC) [22][23][24], which has been demonstrated to be a useful technique for the retention of polar compounds [25]. To the best of our knowledge, only one method has been published for the quantification of varenicline in human plasma, using HPLC-MS/MS preceded by LLE [26], which has then been applied for the study of varenicline pharmacokinetics [27,28].…”

Clinical laboratory testing for smoking toxicity: implications for early identification of respiratory diseases

“…Nicotine metabolites can be tested for in body fluids such as blood, saliva or urine and interestingly such tests are done in research settings, but can be performed at home since point-of-care tests are available in pharmacy stores. 10,11 Perhaps, the debate is; if testing for cigarette toxicity can done at home, why is it not available in the laboratory, where better quality assurance and interpretation of results can be provided. Cigarette toxicity testing is helpful for instance in assessing patients scheduled for surgery or to establish organ transplant eligibility due to increase risk in delayed healing time, infection and thrombosis in nicotine users.…”

Determination of biomarkers of tobacco smoke exposure in oral fluid using solid-phase extraction and gas chromatography–tandem mass spectrometry

“…Several methods have been reported for the determination of NIC, COT and related alkaloids in various biological fluids, and those include immunoassays [18][19][20][21], gas chromatography (GC) coupled to either flame ionisation (FID) [22] or mass spectrometric (MS) detection [1,12,[23][24][25][26], high-performance liquid chromatography (LC) coupled to UV detector [27,28] or MS [7,16,[29][30][31][32][33][34][35][36]. Hydrophilic interaction chromatography-tandem mass spectrometry (HILIC-MS/MS) methods have been also reported [33].…”