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本文建立了猪肉中苯巴比妥残留的Qu ECh ERS气质联用检测方法。样品用乙腈、Mg SO4、醋酸钠提取溶液提取,Mg SO4+PSA+GCB+C18净化,采用毛细管气相色谱柱DB-17(30 m×0.25 mm×0.25μm)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Qu ECh ERS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0.05μg/m L~0.5μg/m L范围内线性关系良好,最低检出限为0.003μg/m L、定量限为0.01μg/m L;在0.01、0.05、0.1μg/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。
This paper established a Qu ECh ERS GC-MS method for the determination of phenobarbital residues in pork. The samples were extracted with acetonitrile, MgSO 4 and sodium acetate extracts and purified by MgSO 4 + PSA + GCB + C 18. The samples were separated by capillary gas chromatography column DB-17 (30 m × 0.25 mm × 0.25 μm) , Determined in selective ion scan (SIM) mode, quantified ions 204 m / z, reference ion 232 m / z, external standard. The selection of conditions such as the acidification of extractant, the type of salt extracted and the type of adsorbent were discussed experimentally. The recoveries of spiked samples were taken as the indexes to optimize the pretreatment conditions of Qu ECh ERS. At the same time, the derivation conditions and matrix effects of the method are discussed. The experimental results showed that phenobarbital had a good linearity in the range of 0.05μg / m L to 0.5μg / m L with the lowest detection limit of 0.003μg / m L and the limit of quantification of 0.01μg / m L; at 0.01,0.05, The recoveries at the concentration of 0.1μg / g ranged from 75.4% to 88.3% and the relative standard deviations (RSD%) ranged from 4.66% to 5.77%. The method is simple and convenient to operate and provides a reference for the detection of sleeping pills in the meat matrix.