A highly efficient polybutylene terephthalate (PBT)-based nanocomposite containing nickel oxide
nanoparticles was synthesized by electrospinning technique and used as a fiber coating for solid phase
microextraction. The influential morphological parameters and capability of the prepared nanocomposite
including the NiO content, the coating time, the PBT concentration and applied voltage were
considered for optimization. The applicability of the synthesized fiber coating was examined by
headspace solid phase micro extraction and gas chromatography mass spectrometry detection of some
volatile organic compounds in aqueous samples. Among the synthesized nanocomposites and pristine
PBT nanofibers, the fiber coating with 14% of NiO nanoparticles doping level exhibited the highest
extraction efficiency. In addition, important parameters influencing the extraction/desorption process
were investigated and optimized. The detection limits were less than 5 ng L1 using the selected ion
monitoring mode. The inter-day and intra-day precisions of the developed method under optimized
conditions were below 11%. The method showed a linearity in the range of 10–1000 ng L1 with the
correlation coefficient greater than 0.9987. The optimized method was applied to the sampling of some
volatile organic compounds from realwater samples. The developed method is convenient, rapid, simple,
easy and inexpensive and offers high sensitivity and sufficient reproducibility