Solid-Phase Microextraction-Based Approach To Determine Free-Base Nicotine in Trapped Mainstream Cigarette Smoke Total Particulate Matter

Abstract

Characterizing nicotine delivery from tobacco products is important in the understanding of their addictive potential. Most previous studies report total nicotine and have not differentiated between nicotine in its protonated or free-base form. Rather than simply determining total nicotine, the method described in this paper determines the amount of free-base nicotine associated with trapped mainstream smoke particulate matter generated using a standardized smoking machine protocol. This method quantitatively determines volatile free-base nicotine associated with the particulate phase portion of mainstream cigarette smoke using solid-phase microextraction combined with gas chromatography-mass spectrometry. The headspace above total particulate matter from mainstream cigarette smoke trapped on a Cambridge filter pad (CFP) was analyzed for free-base nicotine in 26 cigarette brands. The selected cigarette brands were chosen to cover a wide range of tar and nicotine deliveries as measured under Federal Trade Commission machine smoking conditions. In the CFP's headspace the free-base nicotine levels ranged from 0.01 to 0.08 mg/cigarette. The measured ranges of free-base nicotine were remarkably similar over the different tar and nicotine delivery categories of full-flavored, light, and ultralight cigarette brands.

How should we define light or intermittent smoking? Does it matter?

“…This is in contrast to lowtar cigarettes, which allow extraction of higher doses of nicotine and toxins than machine-yield data would suggest ( National Cancer Institute, 2001 ). Cigarettes also vary in their design characteristics, such as their level of fi lter ventilation, which can affect the amount of readily absorbed un-ionized nicotine ( Watson, Trommel, & Ashley 2004 ). Some cigarettes are marketed as containing lower quantities of certain carcinogens and toxins, but studies suggest that reductions in human exposure are less than the reductions reported in the products themselves ( Benowitz, Jacob, Kozlowski, & Yu, 1986 ;Djordjevic, Stellman & Zang, 2000 ;Godtfredsen et al, 2005Godtfredsen et al, , 2006Hatsukami et al, 2006 ;Hecht et al, 2004 ).…”

Measurement of Nicotine in Indoor Air Collected by Alkaline-coated Solid Phase Cartridge Followed by GC-MS Analysis

“…The nitrogen protonation occurs in neutral or acidic conditions. 17) It is believed that protonated nicotine is more adsorptive to the residual silanol groups 18) and more reactive with compounds such as hydroxyl radicals and acidic compounds 19) as compared to free-base nicotine. Therefore, in this study, the modifications to maintain an alkaline condition during the measurement procedure and to prevent the protonation of nicotine were evaluated.…”

An improved headspace solid-phase microextraction method for the analysis of free-base nicotine in particulate phase of mainstream cigarette smoke

“…The 75 m CAR/PDMS fiber was the SPME fiber used by Watson et al [13]. CAR/PDMS fiber usually shows high extraction efficiency for non-or less polar compounds with low molecular weight because of the micro-porosity of Carboxen [21], but has disadvantages such as low selectivity (which usually shows relatively dirty chromatogram) and the need of high temperature for desorption (which can cause carryover and peak tailing problem) [22].…”

“…More recently, Watson et al [13] analyzed the free-base nicotine in mainstream PP smoke of 26 cigarette brands using headspace solid-phase microextraction (HS-SPME) combined with GC/MS. HS-SPME is a simple, sensitive, and solvent-free technique and has been applied for the analysis of many classes of organic compounds in tobacco and cigarette smoke [14][15][16][17][18][19].…”

“…For the same reason, the standard addition calibration method is also not applicable for cigarette smoke sample. Although Watson et al declaimed that toluene-d 8 could be used as an internal standard to compensate for the effect of smoke TPM on the extractability of free-base nicotine by HS-SPME [13], it is reasonable to assume that toluene-d 8 will behave in a markedly different manner than the free-base nicotine during HS-SPME since toluene-d 8 has significantly different properties than free-base nicotine (nonpolar and volatile versus polar and semi-volatile).…”