title: Extraction of toxic compounds from saliva by magnetic-stirring-assisted micro-solid-phase extraction step followed by headspace-gas chromatography-ion mobility spectrometry.
abstract: A new sample extraction procedure based on micro-solid-phase extraction (μSPE) using a mixture of sorbents of different polarities (polymeric reversed-phase sorbent HLB, silica-based sorbent C18, and multiwalled carbon nanotubes) was applied to extract benzene, toluene, butyraldehyde, benzaldehyde, and tolualdehyde present in saliva to avoid interference from moisture and matrix components and enhance sensitivity and selectivity of the ion mobility spectrometry (IMS) methodology proposed. The extraction of target analytes from saliva samples by using μSPE were followed by the desorption step carried out in the headspace vials placed in the autosampler of the IMS device. Then, 200 μL of headspace was injected into the GC column coupled to the IMS for its analysis. The method was fully validated in terms of sensitivity, precision, and recovery. The LODs and LOQs obtained, when analytes were dissolved in saliva samples to consider the matrix effect, were within the range of 0.38-0.49 and 1.26-1.66 μg mL(-1), respectively. The relative standard deviations were <3.5 % for retention time and drift time values, which indicate that the method proposed can be applied to determine toxic compounds in saliva samples. Graphical abstract Summary of steps followed in the experimental set up of this work.
authors.affiliation: Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, University of Córdoba, Annex C-3 Building, Campus of Rabanales, 14071, Córdoba, Spain.
authors.forename: Laura
authors.initials: L
authors.lastname: Criado-García
authors.affiliation: Department of Analytical Chemistry, Institute of Fine Chemistry and Nanochemistry, University of Córdoba, Annex C-3 Building, Campus of Rabanales, 14071, Córdoba, Spain. lourdes.arce@uco.es.
authors.forename: Lourdes
authors.initials: L
authors.lastname: Arce
mesh_terms: D000327:Adsorption; D000328:Adult; D000447:Aldehydes / Q000302:isolation & purification*; D001547:Benzaldehydes / Q000302:isolation & purification*; D001554:Benzene / Q000302:isolation & purification*; D002849:Chromatography, Gas / Q000379:methods; D005260:Female; D006801:Humans; D000075663:Ion Mobility Spectrometry / Q000379:methods; D057230:Limit of Detection; D008280:Magnetics / Q000379:methods; D008297:Male; D037742:Nanotubes, Carbon / Q000737:chemistry; D012463:Saliva / Q000737:chemistry*; D012822:Silicon Dioxide / Q000737:chemistry; D052617:Solid Phase Microextraction / Q000379:methods*; D014050:Toluene / Q000031:analogs & derivatives / Q000302:isolation & purification*
chemical_list: D000447:Aldehydes; D001547:Benzaldehydes; D037742:Nanotubes, Carbon; D014050:Toluene; D012822:Silicon Dioxide; C018475:butyraldehyde; D001554:Benzene; C032175:benzaldehyde
keywords: Ion mobility spectrometry; Micro-solid-phase extraction; Saliva; Toxic compounds