A novel type of nano-carbon composite，magnetic reduced graphene oxide/metal-organic frameworks（MrGO/ZIF－67） was synthesized by combining Fe,3,O,4, nanoparticles with metal-organic framework（ZIF－67） and reduced graphene oxide（rGO），which was employed for the efficient adsorption of methamphetamine（MAMP）．Based on this，a novel ultra-high performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） with magnetic solid phase extraction（MSPE） was established for the rapid determination of MAMP in hair．Scanning electronic microscopy（SEM），transmission electronic microscopy（TEM），Fourier transform infrared spectroscopy（FT－IR） and vibrating sample magnetometer（VSM） were adopted for the comprehensive characterization of MrGO/ZIF－67．The results showed that Fe,3,O,4, magnetic nanoparticles were successfully attached to the surface of carbon composite．MrGO/ZIF－67 possessed a three-dimensional porous structure，multifunctional groups，and sufficient magnetic force for rapid separation by external magnets．A variety of experimental parameters affecting the sample pretreatment effects were evaluated and optimized．The effect of the solution pH value（2.0 to 12.0） was firstly screened by the one-variable-at-a-time（OVAT） analysis，and single factor experiment showed that the solution pH of 11.0 was the most favorable for the adsorption of MAMP．The influences of magnetic nanomaterials amount（1－5 mg），extraction time（10－90 min） and initial concentration of MAMP（100－500 μg/L） on the adsorption performance of MAMP were further investigated via a three level Box-Behnken design and response surface methodology（RSM）．According to the model recommendations，the optimal extraction conditions were as follows：MrGO/ZIF dosage：4 mg，extraction time：20 min，initial concentration of MAMP：110 μg/L．The results showed that there was a good linear relationship for MAMP in the range of 1－200 μg/L，with a correlation coefficient（,r,2,） of 0.999 9，a limit of detection（LOD） of 0.188 μg/L，and a limit of quantitation（LOQ） of 0.572 μg/L．It was found that MrGO/ZIF－67 material had good adsorption capacity，fast adsorption kinetics and easy separation．The spiked recoveries for the actual hair samples at three levels of 1.0，5.0 and 9.6 μg/L ranged from 80.2% to 94.4%，with intra-day and inter-day relative standard deviations（RSDs，,n ,= 3） of 1.6％－2.7% and 6.0%－8.2%，respectively，indicating that the method had good linearity，high sensitivity，good accuracy and precision．The synthesized magnetic nano-carbon composite MrGO/ZIF－67 and the developed UPLC－MS/MS method could be used to adsorb and detect the content of MAMP in actual hair samples.