Differentiation and quantification of xylene isomers by combining headspace solid-phase microextraction/gas chromatography and self-ion molecule reaction in an ion trap tandem mass spectrometry

A headspace solid-phase microextraction (HS-SPME) method using polydimethylsiloxane (PDMS)-coated fiber coupling with GC/self-ion molecule reaction (SIMR)/MS/MS (GC/SIMR/MS/MS) has been developed for the differentiation of o-, m-, and p-xylene isomers. The optimization parameters of this method are: extraction time 20 min, stirring rate 1200 rpm, sampling temperature 28°C, and salt concentration 5%. The LODs were found to be in the range of 3-9 ng/mL under the SIM mode of GC/MS. The RSDs were below 1% (n = 5). The linear dynamic range of the calibration curve was from 0.05 to 10.0 μg/mL with correlation coefficient (r²) > 0.9089. The advantages of this technique are sensitive, selective, ease of operation, simple device, solvent free, and extremely little sample consumption. This technique is the first example using SIMR combined MS/MS applied in the GC/MS and it can be applied to other volatile compounds for future application.