Elsevier

Journal of Chromatography A

Volume 1216, Issue 12, 20 March 2009, Pages 2227-2234
Journal of Chromatography A

Development of an improved method for the determination of polycyclic aromatic hydrocarbons in mainstream tobacco smoke

https://doi.org/10.1016/j.chroma.2009.01.009Get rights and content

Abstract

A gas chromatograph/mass-selective detection (GC/MS) method has been developed and validated for the quantitation of 16 polycyclic aromatic hydrocarbons found in mainstream tobacco smoke condensate. The utilization of two types of solid-phase extraction media combined with capillary column technology removed matrix interferences, afforded a significant reduction in analysis run time, and increased accuracy. Also, the addition of a chilled impinger was used to trap semi-volatile polycyclic aromatic hydrocarbons and to provide more accurate data. This was done without sacrificing the repeatability, reproducibility, and precision obtained in previously published methods. The development and validation studies discussed in this paper resulted in an improved, robust analytical method capable of increasing laboratory capacity and reducing sample reporting time.

Introduction

Polycyclic aromatic hydrocarbons (PAHs) are compounds primarily composed of multiple fused benzene rings formed from the incomplete combustion of organic material (e.g., gas, coal, wood, or tobacco). This diverse class of compounds is composed of semi-volatile and non-volatile compounds of increasing complexity based on the number of rings present in the species, the points of fusion, and the attached functional groups. A few potential sources of PAH exposure are ingestion of grilled, smoked, or fried foods, and from the inhalation of gasoline and diesel exhaust or air pollutants. PAHs are also constituents of tobacco smoke condensate [1], [2], [3], [8], [9].

In the past, the analytical determination of PAHs in mainstream tobacco smoke has presented challenges in obtaining high method precision, accuracy, and sensitivity. In addition, traditional methods for PAH analysis have often been affected by numerous matrix interferences, and have required long analysis run times. Some PAH analytical methods have required large solvent volumes, time-consuming concentration steps, or laborious liquid–liquid extractions [1], [4], [5], [6], [11].

Traditionally, the main PAH of interest in tobacco has been benzo[a]pyrene (B[a]P), which was often used as the benchmark for the entire class of compounds. This analytical method is capable of analyzing 16 PAH compounds of varying molecular weight and structure: naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[e]pyrene, benzo[a]pyrene, indeno[1,2,3-cd]pyrene, and benzo[ghi]perylene. The inclusion of multiple PAHs provides a better representation of the entire class of compounds [7], [9], [12], [13]. The development of this PAH method aimed to reduce the analysis run time and remove matrix interferences, while preserving method precision, accuracy, repeatability, and reproducibility. The effectiveness of the method was validated using Kentucky Reference Cigarettes 3R4F, 1R5F, and Industry Monitor 17 (IM17).

Section snippets

Materials

A custom PAH calibration standard solution (product S-11442-R4) was purchased from Accustandard (New Haven, CT, USA). The internal standards [2H8]naphthalene (naphthalene-d8), [2H10]anthracene (anthracene-d10), [2H12]benz[a]anthracene (benz[a]anthracene-d12), and [2H12]benzo[a]pyrene (benzo[a]pyrene-d12) were obtained from Aldrich (St. Louis, MO, USA) and C/D/N Isotopes (Pointe-Clair, Canada). Solvents used included methanol, cyclohexane, and methylene chloride. All of the solvents were HPLC

Method development

Many published literature methods require the collection of cigarette smoke condensate from twenty or more cigarettes [1], [5], [6], [11]. Increasing the amount of analyte present in a sample is a traditional way to increase sensitivity, but increasing the amount of analyte present in the sample also increases the concentration of the matrix interferences. The higher level of matrix interferences complicates the sample clean-up procedure. The objective of method development was to remove matrix

Conclusion

The development and validation studies yielded a precise, accurate, specific, and sensitive method that demonstrated numerous advantages over previously published methods and is suitable for routine analysis of PAHs in laboratories that lack high-resolution instrumentation. Solid-phase extraction techniques removed many of the matrix interferences, reduced the required number of cigarettes smoked, and increased selectivity and sensitivity. Appropriate capillary column technology afforded a run

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