猪肉中二溴磷残留量的气相色谱和气相色谱/质谱分析

Analysis of Residual Naled in Pork by Gas Chromatography and Gas Chromatography/Mass Spectrometry

试样经盐酸酸化,用正己烷提取残留的二溴磷。提取液在-20℃冷冻2小时凝固析出脂肪,净化液经浓缩定容后,用配有电子俘获检测器的气相色谱测定(GC-ECD),外标定量,并用气相色谱—质谱(选择离子监测)(GC/MS(SIM))进行确证。以HP-5大口径毛细管柱和HP-5MS毛细管柱为分离柱,选择出合适的色谱条件,二溴磷的分离效果良好。本方法对猪肉样品的测定低限为0.05mg/kg;添加浓度为0.05mg/kg～1.00mg/kg时,回收率为89％以上;相对标准偏差小于5.0％;标准进样量在0.1～10.0ng范围内,线性关系良好,r=0.9995。样品前处理采用了微量化学法(MiccM)技术,质谱(选择离子监测)确证的监测离子选m/z 301、185、109amu。

After being acidified with hydrochloric acid, the naled residues in the test sample was extracted with hexane. The extract was stored at-20℃ for 2h to freeze out the fat. The purified solution is concentrated to a defined volume, and analyzed by-GC with electron capture detector (ECD), using external standard method. If necessary, the naled may be confirmed by GC/MS (SIM). HP-5 large internal diameter capillary column and HP-5MS capillary column were used. For a pork sample, the detection limit was 0. 05mg/kg. When the fortifying concentration of naled was in the range of 0. 05mg/kg～1. 00mg/kg, the recovery was more than 89% and the RSD was less than 5.0%. The linearity was favourable when the amount of in jected naled was between 0. 1～10. 0ng, r=0. 9995. The sample extraction was performed according to the microchemical method (MiccM). The m/z 103, 144, 182, 198, 214amu were chosen as MS monitoring ions (SIM).