Stir bar sorptive extraction-thermal desorption-capillary gas chromatography-mass spectrometry applied to the analysis of polychlorinated biphenyls in human sperm.

Stir bar sorptive extraction (SBSE) on polydimethylsiloxane (PDMS) was applied to the enrichment of polychlorinated biphenyls (PCBs) from human sperm. The seven Ballschmiter PCBs were used as model compounds. The extracted PCBs were then thermally desorbed from the stir bar and analysed on-line by capillary gas chromatography (CGC) with mass spectrometric detection (MS). Method development started with the analysis of PCBs spiked in water. Methanol had to be added to the samples in order to reduce the influence of glass adsorption on recovery and reproducibility. Recoveries in water for all PCBs varied around 50-60% and were limited for low molecular mass (MM) PCBs by polarity changes in the sample due to methanol addition and for high MM PCBs by non-equilibrium conditions. Matrix suppression by the lipophilic medium lowered the recoveries in the sperm samples proportional with PCB polarity. The method was validated and although limits of detection (LOD) for the individual congeners were in the sub-ppt level (

Novel preconcentration technique for on-line coupling to high-speed narrow-bore capillary gas chromatography: sample enrichment by equilibrium (ab)sorption. I. Principles and theoretical aspects.

In recent years, there has been substantial progress in the field of high-speed narrow-bore capillary gas chromatography (GC) in general, and in the development of (trans)portable gas chromatographs for fast and accurate analysis in field applications in particular. Due to the limited (concentration) sensitivity of instrumentation for high-speed (portable) GC, environmental applications of this technique frequently require a preconcentration step. The equilibrium (ab)sorption technique described in this article was found to be very promising for on-line coupling to high-speed narrow-bore capillary GC and field portable GC instruments. Enrichment factors up to at least 100 can be obtained rapidly without the use of complicated instrumentation. The new preconcentration technique is shown to have clear advantages over enrichment based on conventional adsorption, i.e. thermal desorption techniques. It can be carried out at ambient trapping temperatures, gives uniform desorption profiles, reduces water effects, uses inert adsorption materials and does not require a (cryogenic) refocusing step. Moreover, the new preconcentration method allows the enrichment factors to be predicted from tabulated chromatographic data, thereby facilitating calibration.

Novel preconcentration technique for on-line coupling to high-speed narrow-bore capillary gas chromatography: sample enrichment by equilibrium (ab)sorption. II. Coupling to a portable micro gas chromatograph.

The technique of equilibrium (ab)sorption has been proven to be a powerful method for preconcentration of gaseous samples for high-speed narrow-bore capillary gas chromatography (GC) in general and field-portable GC instruments, often referred as micro GCs, in particular. Using a simple experimental set-up equipped with an open-tubular enrichment column it is possible to produce a homogeneously enriched sample plug, allowing reproducible injections of an enriched sample into the micro GC. Using a non-polar trapping column enrichment factors found for n-alkanes in the range of C7 to C10 ranged from 15 to 150 and agree well with calculated values. Using a highly retentive Thermocap column, the enrichment factor observed for heptane was above 500. As the use of this new preconcentration method requires only minimum modification of the micro GC, the chromatographic performance of the instrument was not compromised by direct coupling to the preconcentration device. Examples of on-line enrichment with portable micro GC analysis of VOCs from air are shown. These examples clearly demonstrate the potentials of the new method in field analysis.