Analysis of volatile organic compounds (VOCs) is normally preceded by sample homogenization and solvent extraction. This methodology does not provide spatial resolution of the analyzed VOCs in the examined matrix. Here, we present a robotized pen-shaped probe for open-space sampling and mapping of VOCs emanating from solid specimens (dubbed “PENVOC”). The system combines vacuum-assisted suction probe, mass spectrometry, and robotic handling of the probe. The VOCs are scavenged from the sample surface by a gentle hydrodynamic flow of air sustained by a vacuum pump. The sampled gas is transferred to the proximity of corona discharge in an atmospheric pressure chemical ionization source of a tandem mass spectrometer. The PENVOC has been attached to a robotic arm to enable unattended scanning of flat surfaces. The specimens can be placed away from the mass spectrometer during the scan. The robotized PENVOC has been characterized using chemical standards (benzaldehyde, limonene, 2-nonanone, and ethyl octanoate). The limits of detection are in the range from 2.33 × 10–5 to 2.68 × 10–4 mol m–2. The platform has further been used for mapping of VOCs emanating from a variety of specimens: flowers, glove exposed to smoke, fuel stains, worn medical face mask, worn clothing, cheese, ham, and fruits. The chemical maps show unique distributions of the VOCs on the scanned surfaces. Obtaining comparable results (VOC maps) using other techniques (e.g., repetitive headspace sampling prior to offline analysis) would be time-consuming. The presented mapping technique may find applications in environmental, forensic, and food science.
Simultaneous distillation–extraction (SDE) using the Likens–Nickerson apparatus is a convenient technique used to isolate volatile organic compounds (VOCs) from complex liquid matrices. The technique combines steam distillation with solvent extraction. While analytical extractions are normally followed by off-line separation/detection, it is advantageous to couple extractions on-line with separation and detection systems that are employed in the same analytical workflow. Here, we have coupled the Likens–Nickerson apparatus on-line with a gas chromatograph hyphenated with a mass spectrometer. For that purpose, we have devised an automated liquid transfer setup comprising a peristaltic pump, control unit, customized transfer vial with a drain port, and an autosampler arm to deliver liquid extract aliquots at defined time points. The on-line SDE-GC/MS system enables one to record real-time extraction profiles. These profiles reveal extraction kinetics of various VOCs present in the extracted samples. The data sets were fitted with the first order kinetic equation to obtain numeric values characterizing the extraction process (rate constants ranging from 0.21 to 0.01 min–1 for the ethyl esters from C6 to C19). A comparison of on-line and off-line results reveals that the on-line system is more dependable, while the off-line analysis leads to artifacts. To demonstrate the operation of the on-line SDE-GC/MS system, we performed analyses of selected real samples (beer). The real-time data sets revealed extraction kinetics for VOCs present in these samples. The devised extraction-analysis system allows the analysts to make an evidence-based decision on the extraction time for different groups of analytes in order to maximize extraction yield and minimize analyte losses.
The occurrence of crimes involving high explosives in Malaysia in recent years has warrant the need for the analysis of high explosives in post blast samples, particularly residues that could be found on hairs of victims. This study reports on the detection of post blast residues of C4 explosives on human head hairs. Prior to a simulated explosion, a bundle of hair (200 strands) was tightly bound to a metal hook at each point of several pre–determined distances from the bomb seat. Hair samples containing post blast residues were extracted by ultrasonication using acetonitrile. Two analytes of interest, cyclotrimethylenetrinitramine (RDX) and pentaerythritol tetranitrate (PETN) were successfully separated using gas chromatography with electron capture detector (GC–ECD) on an HP5–MS capillary column. It was found that the amount of explosive residues decreased with increasing distance from the point of blast. At the nearest specified distance of 2.5m, the amount of PETN residues deposited on hair was much less compared to that of RDX residues.
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