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The objective of this study is determination the volatile compounds of Matricaria chamomilla of an inorganic–organic hybrid material based on ZnO nanoparticles anchored to a composite made from polythiophene and hexagonally ordered silica (ZnO/PT/SBA-15) as a solid-phase fiber microextraction (SPME). Microextraction techniques with nanoparticles ZnO/PT/SBA-15 resulted in a more efficient analyte enrichment, faster sample preparation, and lower solvent consumption. Furthermore, they are simple, inexpensive, environmentally friendly, and compatible with many analytical instruments. Using ZnO/PT/SBA-15 followed by GC–MS, 37 compounds were separated and identified in Matricaria chamomilla, which mainly included α-bisabolol(17.51%), Cis-trans-farneso(8.72%), β-bisabolene(8.37%), E-β–Farnesene(5.48%) Guaiazulene(4.36%), α-Pinene(3.68%) and Limonene(3.24%). The presented experimental results clearly demonstrate that prepared fibers are suitable for SPME analyses of volatile oils. For optimization of the microextraction conditions by the ZnO/PT/SBA-15 SPME fiber, a one at the time optimization strategy was used. The optimized parameters were sample state and its amount, extraction temperature and time and finally desorption conditions.