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A novel miniaturized sample extraction capillary was developed to provide a simple and sensitive method for analyzing gaseous formaldehyde (FA) using conventional high-performance liquid chromatography (HPLC). The extraction capillary was prepared by packing silica gel particles in a stainless steel capillary with a 1.6-mm o.d. Before the gaseous samples were collected, the silica gel particles were impregnated with a derivatizing reagent 2,4-dinitrophenylhydrazine (DNPH) by passing a solution of DNPH through the extraction capillary. FA was derivatized to form the corresponding hydrazone during the active sampling of a gaseous sample, and the derivative was sorbed by the silica gel. The capillary was then directly connected to a six-port valve, and desorption from the capillary and injection into the HPLC were achieved simultaneously by passing a solvent through the capillary. The run-to-run and device-to-device variabilities, as relative standard deviations, were both less than 6.9 %. The limit of detection for FA was 2.5 ng/L using a sampling volume of 100 mL, and a sample collection time of 2 min. Acetaldehyde and acetone in a gaseous sample could also be simultaneously extracted and determined using this method. The applicability of the developed method for determining FA in real indoor air samples was confirmed by comparing the results obtained using the proposed method and a conventional sample preparation method. The developed method enables the rapid and simple sample preparation of gaseous FA and gives a good level of sensitivity. [ABSTRACT FROM AUTHOR]

• Miniaturized sample preparation with braid-type extraction medium was developed. • The extraction capillary was prepared using the braid with a metal wire inside. • Applying low voltages to the metal wire, a heat-assisted desorption was made. A novel miniaturized sample preparation device with braid-type extraction medium was successfully developed. Introducing a set of bundles of fine synthetic filaments as the materials of the braid-type extraction medium and also the application of an appropriate tension during the braiding process, the outer diameter of the resulting braid has been controlled. Optimization of the tension enables an easy preparation of a group of braids that can be well-compatible to various internal diameters of capillaries to be packed. The extraction conditions were systematically optimized, and the efficient extraction was confirmed under the optimized conditions. All the parameters affects the desorption efficiency were also optimized, where typical extraction efficiency was more than 90% for the extraction of phenanthrene (1.0 μg/mL) in water. The extracted analyte was desorbed sufficiently by employing a sequential pumping process of two organic solvents. During the preparation of the braid, a different type of fibrous materials could be inserted to the opening at the center of the braid. Taking advantage of this feature of the braid, a stainless steel wire was inserted into the center of the braid. By applying low voltages to the stainless steel wire, a heat-assisted desorption of the extracted analyte was also studied. Experimentally complete desorption (higher than 99.0%) was obtained with the voltage application of 2 V. The lowest limit of quantification (LOQ) and the lowest limit of detection (LOD) for phenanthrene were 0.048 and 0.014 μg/mL, respectively. [ABSTRACT FROM AUTHOR]