在固相萃取柱，样品提取溶剂及淋洗液体积的选择基础上，建立了水果中36种农药残留的气相色谱-质谱法(GC/MS)检测方法。水果样品经乙腈提取，采用石墨化碳黑/氨基柱(PC/NH2)净化后，用GC/MS单离子监测扫描模式(SIM)进行检测，基质匹配溶液外标法定量。各个目标物在70.00 ng/mL~560.0 ng/mL范围内呈良好的线性相关，相关系数(R2)均不小于0.990，方法的检出限(LOD，S/N=3)为0.0001~0.0018 mg/kg，定量限(LOQ，S/N=10)为0.0002~0.0060 mg/kg。分别在提子基质中做低、中、高3个添加水平的加标回收试验，该方法的平均回收率为60.6%~116.5%，相对标准偏差RSD(n=6)在0.8%~9.5%之间。该方法前处理步骤简便，基质经固相萃取柱净化后的效果满意，特异性更强，适用范围广，适用于仁果类及小型攀缘类水果中多组分农残的筛查和确证工作。

A gas chromatography-mass spectrometry (GC/MS) method for the determination of 36 pesticide residues in fruits was established on the basis of the selection of solid phase extraction column, extraction solvent and eluent volume. The fruit samples were extracted with acetonitrile, purified by graphitized carbon black/amino solid-phase column (PC/NH2) t, analyzed by GC/MS with the single ion monitoring scanning mode (SIM), and quantified by the matrix-matched method with external standards. All the targeted substances showed a good linear correlation in the range of 70.00 ng/mL~560.0 ng/mL, with the correlation coefficients (R2) not less than 0.990. The limit of detection (LOD) of the method ranged in 0.0001~0.0018 mg/kg when the signal/noise (S/N) ration =3, with the limit of quantification (LOQ) in the range of 0.0002~0.0060 mg/kg (S/N=10). The spiked recovery tests were carried out at low, medium and high levels of the extraction matrix. The average recovery of the method ranged in 60.6 %~116.5 % with the relative standard deviations (RSDs, n=6) in the range of 0.8%~9.5%.The results demonstrated that the method is simple and the outcome of purification of matrix by solid phase extraction was satisfactory. Owing to high specificity and broad range of application, this method is suitable for screening and verification of multicomponent pesticide residues in pome fruits and small climbing fruits.

贵州省科技支撑计划项目（黔科合支撑[2017]2890）；贵州省高层次创新型人才百层次人才（贵州省科技厅黔科合人才[2015]4029号）；贵州省科技创新团队（黔科合人才团队[2015]4025号）；贵州省高等学校科技创新人才团队（黔教合人才团队字[2014]31）