Abstract:Objective: A solid phase extraction-gas chromatography/mass spectrometry (GC-MS) method was developed for the simultaneous determination of 24 pesticide residues in coffee peel. Methods: The sample was wetted with water, extracted with acetonitrile, the extract solution is concentrated and then purified with ProElut TPC solid phase extraction column, eluted with acetonitrile and toluene=3∶1, after concentration, the sample was determinated by GC-MS and the peak area was measured by internal standard method. Results: The 24 pesticides were separated well within 28 minutes. The residue of pesticide was in the range of 0.016~0.400 mg/kg, the linearity of the method was good, the correlation coefficient r was between 0.997 9~0.999 9, the quantitative limit was between 0.01~0.03 mg/kg, when the concentration of pesticide is 0.03 mg/kg and 0.30 mg/kg, the recovery rate is between 65.2%~108.5% and 81.4%~105.7%, The relative standard deviation of intra day precision is between 3.7%~6.8% and 2.5%~5.9%, and the relative standard deviation of daytime precision is between 4.2%~7.2% and 2.8%~6.4%, compared with acetonitrile∶toluene=3∶1, as eluting solvent and ProElut TPC as purification column, the elution and purification efficiency were the highest, and the recovery was 95%. Conclusion: The performance parameters of the method meet the requirements of national standards, and the determination results are accurate and reliable. It can be applied to the qualitative and quantitative analysis of multi-component pesticide residues in dried coffee peel.