Journal of Chromatography A, 1219 (2012) 180–187 Contents lists available at SciVerse ScienceDirect Journal of Chromatography A journal homepage: www.elsevier.com/locate/chroma Determination of nicotine and N-nitrosamines in house dust by pressurized liquid extraction and comprehensive gas chromatography—Nitrogen chemiluminiscence detection Noelia Ramírez a , Mustafa Z. Özel b , Alastair C. Lewis c , Rosa M. Marcé a,∗ , Francesc Borrull a , Jacqueline F. Hamilton b a Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Marcel·lí Domingo s/n, Sescelades Campus, Tarragona 43007, Spain b The University of York, Department of Chemistry, Heslington, York YO10 5DD, UK c National Centre for Atmospheric Science, The University of York, Department of Chemistry, Heslington, York YO10 5DD, UK article info Article history: Received 27 September 2011 Received in revised form 8 November 2011 Accepted 10 November 2011 Available online 15 November 2011 Keywords: Nicotine Tobacco-specific nitrosamines (TSNAs) House dust Comprehensive gas chromatography (GC × GC) Nitrogen chemiluminiscence detector (NCD) Pressurized liquid extraction (PLE) abstract A novel, highly selective method for the determination of nicotine, N-nitrosamines and tobacco-specific nitrosamines (TSNAs) in indoor dust samples is presented in this study. Samples were extracted by in-cell clean-up pressurized liquid extraction (PLE) that allows high extraction efficiency with moderate con- sumption of organic solvents. The extracts were analyzed by comprehensive gas chromatography and detected with a nitrogen chemiluminiscence detector (GC × GC-NCD) that provided enhanced selectivity and sensitivity for organic nitrogen containing compounds. Method validation showed good linearity, repeatability and reproducibility (%RSD < 8%). Recovery was higher than 80% for most target com- pounds and limits of detection lower than 16 ng g -1 . The method was used for the determination of the nitrosamine target compounds in house dust samples from both smoking and non-smoking households. All the analytes were found in the samples, nicotine being the most abundant compound in smokers’ dust and one of the most abundant in non-smokers’ dust. To our knowledge this is the first time that volatile N-nitrosamines and TSNAs have been determined in indoor dust samples. The results demonstrate the presence of these highly carcinogenic compounds in house dust, with inherent human exposure through inhalation and/or involuntary ingestion of house dust. © 2011 Elsevier B.V. All rights reserved. 1. Introduction House dust has been identified as a major source of envi- ronmental contaminants including pesticides, polycyclic aromatic hydrocarbons (PAHs), phthalates, several metals, and other chem- icals of human health concern [1,2]. Since contaminants bound to indoor dust are more persistent than those outdoors, indoor dust has been recognized as a significant source of human exposure for an increasing number of pollutants. For instance, the ingestion of house dust has been estimated to be the major route of exposure to some persistent pollutants for children [3]. Furthermore, recently, it has been demonstrated that indoor dust may be the main route of exposure to polybrominated diphenyl ethers for both adults and children [4]. House dust is therefore a key pollutant vector and one which demands further examination for the presence of other contaminants of human health concern. ∗ Corresponding author. Tel.: +34 977 55 81 70; fax: +34 977 55 84 46. E-mail address: rosamaria.marce@urv.cat (R.M. Marcé). One of the most important sources of indoor pollution is tobacco smoke. Nicotine is the most abundant organic compound emit- ted during smoking [5]. It reacts during the burning of tobacco to form tobacco-specific nitrosamines (TSNAs). TSNAs are amongst the most abundant carcinogenic compounds identified in tobacco smoke [6] and they have been related to acute leukemia [7] and lung cancer [8]. Of all TSNAs identified, N ′ -nitrosonornicotine (NNN) and 4-(methylnitrosoamino)-1-(3-pyridyl)-1-butanone (NNK) are the most prevalent carcinogens in tobacco products and are classified as carcinogenic for humans (Group 1 IARC) [9]. Another interesting TSNA is 4-(methylnitrosoamino)-1-(3-pyridyl)-1-butanol (NNAL), which is the main metabolite of NNK and has the same dan- gers [10]. Moreover, more volatile N-nitrosamines, with genotoxic and carcinogenic properties can be formed in the atmosphere because of the presence of nitrogen-containing species origi- nating during combustion processes [11]. Some studies have also detected the presence of volatile N-nitrosamines, such as N-nitrosodimethylamine and N-nitrosopyrrolidyne, in environ- mental tobacco smoke [12,13]. Nicotine deposits almost entirely on indoor surfaces and per- sists for long time [14,15]. This deposited nicotine can also form 0021-9673/$ – see front matter © 2011 Elsevier B.V. All rights reserved. doi:10.1016/j.chroma.2011.11.017