A new design of hyperbranched polyglycerol/graphene oxide nanocomposite reinforced hollow fibersolid/liquid phase microextraction (HBP/GO −HF-SLPME) coupled with high performance liquid chro-matography used for extraction and determination of ibuprofen and naproxen in hair and waste watersamples. The graphene oxide first synthesized from graphite powders by using modified Hummersapproach. The surface of graphene oxide was modified using hyperbranched polyglycerol, through directpolycondensation with thionyl chloride. The ready nanocomposite later wetted by a few microliter ofan organic solvent (1-octanol), and then applied to extract the target analytes in direct immersion sam-pling mode.After the extraction process, the analytes were desorbed with methanol, and then detectedvia high performance liquid chromatography (HPLC). The experimental setup is very simple and highlyaffordable. The main factors influencing extraction such as; feed pH, extraction time, aqueous feed vol-ume, agitation speed, the amount of functionalized graphene oxide and the desorption conditions havebeen examined in detail. Under the optimized experimental conditions, linearity was observed in therange of 5–30,000 ng mL−1for ibuprofen and 2–10,000 ng mL−1for naproxen with correlation coeffi-cients of 0.9968 and 0.9925, respectively. The limits of detection were 2.95 ng mL−1for ibuprofen and1.51 ng mL−1for naproxen. The relative standard deviations (RSDs) were found to be less than 5% (n = 5).

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