For the fast and selective preconcentration-separation of carbaryl from environmental samples, a simple and cheap supramolecular solvent microextraction method (Ss-ME) has been applied with ultra-performance liquid chromatography-tandem mass spectrometry. Various analytical parameters that have a noticeable effect on the extraction of carbaryl by supramolecular liquid phase microextraction were optimised by selecting the peak area as the response. The parameters including pH of solution, type and volume of supramolecular formula, matrix effect and the sample volume were optimised. The quantitative recoveries were obtained between pH 2.0 and 4.0 of sample solution phase by using a supramolecular phase consist of heptanol and tetrahydrofuran. The limit of detection and limit of quantification were 0.03 mg L-1 and 0.09 mg L-1 respectively. The relative standard deviation was 7.11 and the preconcentration factor was 15. The microextraction procedure for trace carbaryl was used for various samples such as fruits, vegetables and water samples with the recovery% range between 90% and 102%.