气相色谱-串联质谱检测鹅组织中哌嗪残留

发布时间：2019-05-28 14:15

【摘要】：建立了鹅组织(肌肉、肝脏、肾脏以及皮肤和脂肪)中哌嗪残留的气相色谱-串联质谱检测法。鹅组织经加速溶剂萃取(ASE350),乙腈提取,过Strata-X-C固相萃取小柱净化后的样品在乙酸酐和三乙胺条件下衍生。衍生产物经气相色谱-串联质谱仪(GC-MS/MS)检测,色谱柱为TG-5MS Amine(30 m×0.25 mm i.d.,0.25μm),载气为氦气,进样口和检测器温度均为280℃。采用EI模式,SCAN和SIM扫描定性,Auto SRM结合外标法定量。哌嗪添加量在5.1~2.5×10~3μg/kg范围内,线性关系良好,相关系数为0.9995。在定量限(LOQ:5.1,5.2,5.2,5.2)~2.0×10~3μg/kg的加标水平上,鹅组织中哌嗪的平均回收率为85.2%~95.5%,相对标准偏差(RSD)为1.6%~4.7%,日内RSD为1.2%~5.3%,日间RSD为2.0%~7.7%。检测限(LOD)和定量限(LOQ)分别在1.4~1.6μg/kg(S/N≥3)和5.1~5.2μg/kg(S/N≥10)之间。方法适用于鹅组织中哌嗪残留的检测。
[Abstract]:A gas chromatography-tandem mass spectrometry (GC-MS) method for the determination of piperazin residues in goose tissues (muscle, liver, kidney, skin and fat) was established. The samples purified by accelerated solvent extraction (ASE350), acetonitrile extraction and Strata-X-C solid phase extraction column were derived from goose tissue under the conditions of acetic anhydride and triethylamine. The derived products were detected by gas chromatography-tandem mass spectrometry (GC-MS/MS). The chromatographic column was TG-5MS Amine (30 m 脳 0.25 mm I.D., 0.25 渭 m), the carrier gas was Helium, and the injection port and detector temperature were 280 鈩，

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