Automatic heating and cooling system in a gas purge microsyringe extraction

Abstract

The gas purge microsyringe extraction (GP-MSE) technique offers quantitative and simultaneous extraction, and rapid gas chromatographic-mass spectrometric determination of volatile and semivolatile chemicals is possible. To simplify the application, a new automatic temperature control system was developed here. Stable heating and cooling over a wide range of temperatures were achieved using a micro-heater and thermoelectric cooler under varying gas flow conditions. Temperatures could be accurately controlled in the range 20-350°C (heating) and 20 to -4°C (cooling). Temperature effects on the extraction performance of the GP-MSE were experimentally investigated by comparing the recoveries of polycyclic aromatic hydrocarbons (PAHs) under various experimental conditions. A sample treatment was completed within 3 min, which is much less than the time required for chromatographic analysis. The recovery of chemicals determined ranged from 81 to 96%. High reproducibility data (RSD ≤ 5%) were obtained for direct extraction of various analytes in spiked complex plant and biological samples. The data show that the heating and cooling system has potential applications in GP-MSE system for the direct determination of various kinds of volatile and semivolatile chemicals from complex matrices without any, or only minor, sample pretreatment.