Improved pre-concentration and detection methods for volatile sulphur breath constituents

摘要

Suitability of different types of pre-concentration (solid phase microextraction and sorbent trapping) and detection (flame photometric detector (FPD) and mass selective detector (MSD)) for gas chromatographic determination of sulphur-containing compounds (H2S, MeSH, EtSH, DMS, COS and CS2) in breath-gas was assessed in this study. Several factors like influence of humidity, influence of oxygen, or stability of target compounds in extraction vessels (SPME vials and sorbent tubes) were investigated. Despite poor stability of VSCs in SPME vials and matrix effects (unfavorable influence of humidity), SPME was found to be a fast and reliable enrichment method, which coupled with mass selective detector provided satisfactory LODs of target compounds at the ppt level (from 0.15 ppb for CS2 to 2.3 ppb for H2S). Application of sorbent trapping with two-bed sorbent tubes containing Tenax TA and Carboxen 1000 gave excellent LODs (0.03-0.3 ppb for 200 ml sample and MSD). Stability of investigated VSCs in sorbents was found to be very poor (30-40% losses after 2 h). FPD showed satisfactory sensitivity only when it was coupled with sorbent trapping. Breath samples were collected into Tedlar bags in a CO2-controlled manner. Humidity was removed during sampling (permeation dryer - Nafion) to avoid unfavorable water dependent effects during analysis.