The present work was designed with the aim to one step simple hydrothermal synthesis of moss like MWCNT-Bi2S3 nanomaterial as solid phase extraction sorbent for separation, preconcentration and determination of copper in tobacco and food samples. Cu(II) ions was strongly retained on the MWCNT-Bi2S3 nanomaterial at the pH 7.0 and was successfully desorbed by using 1.5 mL of 4 M HNO3. The copper concentration in eluent was determined by flame atomic absorption spectrometer. The certified reference material (NC SZC 73033 Scallion) was analyzed for the verification and accuracy of the proposed method. This work was interpreted statistically and found the analytical performance of the proposed method which consist of preconcentration factor (20), limit of quantification (13.1 pg L(-)1) and relative standard deviation (2.2%), respectively. It was concluded that this method was applied for the detection of copper from different types of tobacco and food samples successfully.