Abstract

Active and passive smoking are serious public health concerns Assessment of tobacco smoke exposure using effective biomarkers is needed. In this study, we developed a simultaneous determination method of five tobacco-specific nitrosamines (TSNAs) in hair by online in-tube solid-phase microextraction (SPME) coupled to liquid chromatography-tandem mass spectrometry (LC–MS/MS). TSNAs were extracted and concentrated on Supel-Q PLOT capillary by in-tube SPME and separated and detected within 5 min by LC–MS/MS using Capcell Pak C18 MGIII column and positive ion mode multiple reaction monitoring systems. These operations were fully automated by an online program. The calibration curves of TSNAs showed good linearity in the range of 0.5–1000 pg mL–1 using their stable isotope-labeled internal standards. Moreover, the limits of detection (S/N = 3) of TSNAs were in the range of 0.02–1.14 pg mL–1, and intra-day and inter-day precisions were below 7.3% and 9.2% (n = 5), respectively. The developed method is highly sensitive and specific and can easily measure TSNA levels using 5 mg hair samples. This method was used to assess long-term exposure levels to tobacco smoke in smokers and non-smokers.

Highlights

  • Active and passive smoking are serious public health concerns because they increase the risk of various cancers, cardiovascular diseases and respiratory diseases [1,2]

  • The present study describes the development of an online in-tube solid-phase microextraction (SPME) LC–MS/MS method for the simultaneous determination of five tobacco-specific nitrosamines (TSNAs), including NNAL, in hair samples and applying this method to the assessment of tobacco smoke exposure in smokers and non-smokers

  • We previously described the optimization of in-tube SPME conditions for four TSNAs, excluding NNAL [24]

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Summary

Introduction

Active and passive smoking are serious public health concerns because they increase the risk of various cancers, cardiovascular diseases and respiratory diseases [1,2]. In-tube SPME, using an open tubular capillary column with an inner surface coating as an extraction device, is an efficient sample preparation method that allows automation of the extraction and concentration process and can be coupled online to HPLC or LC–MS system using column switching technique [25,26,27] It reduces the use of and exposure to harmful organic solvents and reduces analysis times and gives higher sensitivity and good precision. The present study describes the development of an online in-tube SPME LC–MS/MS method for the simultaneous determination of five TSNAs, including NNAL, in hair samples and applying this method to the assessment of tobacco smoke exposure in smokers and non-smokers

Optimization of In-Tube Solid-Phase Microextraction and Desorption of TSNAs
Analytical Method Validation
Application to the Analysis of Hair Samples
Reagents and Standard Solutions
Preparation of Hair Samples
In-Tube SPME
Conclusions
Full Text
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