Relevance. The need for sensitive determination of the content of higher alcohols in water and water-oil emulsions to solve hydrological problems and tracer studies of oil deposits. Aim. Minimization of sample preparation in the gas chromatographic determination of higher alcohols based on the use of macrocyclic glycoluryl derivatives as a new sorption material. Methods. Gas chromatography, thermogravimetry, statistical methods. Results and conclusions. The authors have developed new sorbents based on the Chromaton N-AW DMCS solid carrier and macrocyclic glycoluryl derivatives in combination with fixed liquid phases OV-101, SE-52 and CBWX 20M for microextraction. The paper shows practical application of an environmentally friendly analytical technique for the gas chromatographic determination of higher alcohols in water bodies. The validation of the method was performed using calibration and minimization of matrix effect. The proposed method demonstrated low detection and quantification limits, 1,5 and 4,5 mg/L, respectively, while the accuracy of the method did not exceed 10%. At the stage of microextraction of higher alcohols, the extraction rate was >94%. The use of mixtures of macrocyclically produced glycoluryl with fixed liquid phases OV-101, SE-52 and CBWX 20M for gas chromatographic separation and identification showed a resolution of high alcohols with hydrocarbons >1.12, which confirms the selectivity of their separation. The authors studied the textural and chromatographic properties of new sorption materials, determined the thermal stability range of macrocyclic glycoluryl derivatives and the maximum operating temperature of sorbents. The paper demonstrates the possibility of practical application of the obtained new sorption materials for microextraction and gas chromatographic express determination of higher aliphatic alcohols C3-C12 at sufficiently low detection and quantification limits.