Development and Application of Porous Membrane-Protected Carbon Nanotube Micro-Solid-Phase Extraction Combined with Gas Chromatography/Mass Spectrometry

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Abstract
A novel, multiwalled carbon nanotube (MWCNT)-supported micro-solid-phase extraction (μ-SPE) procedure has been developed. A 6-mg sample of MWCNTs was packed inside a (2 cm × 1.5 cm) sheet of porous polypropylene membrane whose edges were heat-sealed to secure the contents. The μ-SPE device, which was wetted with dichloromethane, was then placed in a stirred sewage sludge sample solution to extract organophosporous pesticides, used here as model compounds. Tumbling of the extraction device within the sample solution facilitated extraction, and the porous membrane acted as a filter to exclude the extraction of extraneous materials. After extraction, analytes were desorbed in hexane and analyzed using gas chromatography/mass spectrometry. Since the porous membrane afforded protection of the MWCNTs, no further cleanup of the extract was required. The π−π electrostatic interaction with the analytes and the large surface area of MWCNTs facilitated the adsorption of analytes, with good selectivity and reproducibility. Under the optimized extraction conditions, the method showed good linearity in the range of 0.1−50 μg/L, repeatability of the extractions (RSD 2−8%, n = 4), and low limits of detection (1−7 pg/g). No analyte carryover effect was observed, and each μ-SPE device could be used for up to 30 extractions. Comparison was made with hollow fiber protected solid-phase microextraction and headspace solid-phase microextraction; μ-SPE was demonstrated to be a fast, accurate, and cost-effective pretreatment method for sewage sludge samples.