Carbamate pesticides is one of the most dangerous organic compounds in the environment. In parallel with strict regulation and control of organic contaminants, there is an emerging trend of analytical determination and development towards finding an environmentally friendly pre-concentration technique. Microextraction methods are steps in this direction. In the current study, a new FND-CHF polar sorbent was proposed for the extraction of carbamate pesticides from aqueous medium. The functional groups on the nanodiamonds which have higher electrostatic interaction with the target analytes enhance the efficiency of this method as compared to the unmodified polypropylene hollow fiber. The factors that affect the preconcentration efficiency were studied and optimized. Gas chromatography-Mass spectrometry (GC-MS) technique was selected to determine the target analytes after on-column derivatization. Under the optimum conditions, the extraction efficiency of the novel method was high, with detection limits in the range of 0.044 to 0.084 µg.L-1. The reproducibility of extraction devices used for these experiments was satisfactory (relative standard deviations ranged from 3.4% to 7.7%). This indicates that this technique is excellent for routine analysis of environmental samples. The proposed novel technique gives an added advantage of reducing solvent consumption. Furthermore, the devices are inexpensive and can be prepared easily.