本文建立了猪肉中苯巴比妥残留的QuEChERS气质联用检测方法。样品用乙腈、MgSO4、醋酸钠提取溶液提取，MgSO4+PSA+GCB+C18净化，采用毛细管气相色谱柱DB-17（30 m×0.25 mm×0.25 μm）分离，电子轰击电离源（EI），在选择离子扫描（SIM）模式下测定，定量离子204 m/z、参考离子232 m/z，外标法定量。实验对提取剂是否酸化、提取盐种类以及吸附剂种类等条件的选择进行了讨论，并以加标回收率作为考察指标，优化了QuEChERS的前处理条件。同时，讨论了方法的衍生条件及基质效应。实验表明，苯巴比妥在0.05 μg/mL~0.5 μg/mL范围内线性关系良好，最低检出限为0.003 μg/mL、定量限为0.01 μg/mL；在0.01、0.05、0.1 μg/g添加水平下回收率在75.4%~88.3%之间，相对标准偏差（RSD%）介于4.66%~5.77%之间。 该方法操作简单、方便，为肉类基质中的安眠药类残留检测提供了参考。

A novel method for the detection of phenobarbital residue in pork using gas chromatography–mass spectrometry (GC-MS) combined with the “Quick, Easy, Cheap, Effective, Rugged and Safe” (QuEChERS) was established here. The analytes were extracted using acetonitrile, MgSO4, and NaAc solutions and purified with MgSO4+PSA+GCB+C18 adsorbents. The samples were then separated on a DB-17 capillary column (30 m × 0.25 mm × 0.25 μm) and the ion source was electron ionization (EI). The target compound was detected in the selected ion monitoring (SIM) mode; the quantitative ion was 204 m/z, the reference ion was 232 m/z, and external standard calibration was used for the quantitative analysis of phenobarbital. To optimize the pretreatment for QuEChERS, conditions such as acidification of the extraction solution, choices of extraction salts, and adsorbent type were discussed using the spike-recovery rate as the evaluation index. The derivative conditions and matrix effects were discussed as well. The results indicated that phenobarbital had satisfactory linearity from 0.05 to 0.5 μg/mL. The limit of detection (LOD) was 0.003 μg/mL and the limit of quantitation (LOQ) was 0.01 μg/mL. The recovery rates at three spiking levels (0.01, 0.05, and 0.1 μg/g) were 75.4% to 88.3%, and the relative standard deviations were 4.66% to 5.77%. The QuEChERS method combined with GC-MS was simple and convenient, which may provide a reference method for detecting hypnotic residues in meat matrix.

质检公益性行业专项资助项目（201110207）