title: Needle trap micro-extraction for VOC analysis: effects of packing materials and desorption parameters.
abstract: Combining advantages of SPE and SPME needle trap devices (NTD) represent promising new tools for a robust and reproducible sample preparation. This study was intended to investigate the effect of different packing materials on efficacy and reproducibility of VOC analysis by means of needle trap micro extraction (NTME). NTDs with a side hole design and containing different combinations of PDMS, DVB and Carbopack X and Carboxen 1000 and NTDs containing a single layer organic polymer of methacrylic acid and ethylene glycol dimethacrylate were investigated with respect to reproducibility, LODs and LOQs, carry over and storage. NTDs were loaded with VOC standard gas mixtures containing saturated and unsaturated hydrocarbons, oxygenated and aromatic compounds. Volatile substances were thermally desorbed from the NTDs using fast expansive flow technique and separated, identified and quantified by means of GC-MS. Optimal desorption temperatures between 200 and 290°C could be identified for the different types of NTDs with respect to desorption efficiency and variation. Carry over was below 6% for polymer packed needles and up to 67% in PDMS/Carboxen 1000 NTDs. Intra and inter needle variation was best for polymer NTDs and consistently below 9% for this type of NTD. LODs and LOQs were in the range of some ng/L. Sensitivity of the method could be improved by increasing sample volume. NTDs packed with a copolymer of methacrylic acid and ethylene glycol dimethacrylate were universally applicable for sample preparation in VOC analysis. If aromatic compounds were to be determined DVB/Carboxen 1000 and DVB/Carbopack X/Carboxen 1000 devices could be considered as an alternative. PDMS/Carbopack X/Carboxen 1000 NTDs may represent a good alternative for the analysis of hydrocarbons and aldehydes. NTME represents a powerful tool for different application areas, from environmental monitoring to breath analysis.
authors.affiliation: Department of Anaesthesia and Intensive Care, University of Rostock, Rostock, Germany.
authors.forename: Phillip
authors.initials: P
authors.lastname: Trefz
authors.forename: Sabine
authors.initials: S
authors.lastname: Kischkel
authors.forename: Dietmar
authors.initials: D
authors.lastname: Hein
authors.forename: Ellwood Sean
authors.initials: ES
authors.lastname: James
authors.forename: Jochen K
authors.initials: JK
authors.lastname: Schubert
authors.forename: Wolfram
authors.initials: W
authors.lastname: Miekisch
mesh_terms: D000327:Adsorption; D005591:Chemical Fractionation / Q000295:instrumentation* / Q000379:methods*; D004129:Dimethylpolysiloxanes; D008401:Gas Chromatography-Mass Spectrometry; D057230:Limit of Detection; D008689:Methacrylates; D009339:Needles; D015203:Reproducibility of Results; D013696:Temperature; D014753:Vinyl Compounds; D055549:Volatile Organic Compounds / Q000032:analysis / Q000302:isolation & purification*
chemical_list: D004129:Dimethylpolysiloxanes; D008689:Methacrylates; D014753:Vinyl Compounds; D055549:Volatile Organic Compounds; C008384:methacrylic acid; C013830:baysilon; C004919:ethylene dimethacrylate; C004985:divinyl benzene