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气相色谱法测定动物性食品中辛硫磷残留量

     

摘要

The method based on GC was developed for the determination of phoxim residue in liver and muscle tissues of pig, cattle, sheep and chicken. The samples were extracted by acetonitrile after dehydrated with anhydrous sodium sulfate. The residue was dissolved with acetone, filtered by 0.45 p,m filter membrane and detected by GC after dried by rotary evaporators. The result was quantified by external standard method. The calibration curve was in good linearity between the peak area and the concentration of 0.10 - 2.00 p.g/ml for phoxim with R2 >0.9990. The detection limits of phoxim was 15 p,g/kg, and the quantification limits was 40 jig/kg. The average recovery rate ranged from 75.7% to 99.0% at the additive concentration of 40, 50 and 100 ug/kg. The relative standard deviations of intra - and inter - batch were both less than 12%. In conclusion, the technology for detecting phoxim residue was convenient, rapid, reliable and accurate with high sensitivity.%建立了气相色谱法测定猪、牛、羊、鸡的肝脏和肌肉组织中辛硫磷残留量的检测方法.样品经无水硫酸钠脱水,用乙腈提取,提取液55℃水浴下旋转蒸发至近干,残留物用丙酮溶解,0.45 μm滤膜过滤后经气相色谱仪检测,外标法定量.辛硫磷标准溶液在0.10~2.00 μg/ml范围内呈良好的线性关系,R2均大于0.999,方法检出限为15 μg/kg,最低定量限为40 μg/kg,在40、50、100 μg/kg添加水平上,添加回收率为75.7%~99.0%,批内、批间RSD均小于12%.该残留检测方法具有前处理简便、快速、灵敏度高、选择性好等优点.

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