高效液相色谱法测定动物性食品中辛硫磷残留量的研究

Determination of Phoxim Residues in Animal Derived Food by HPLC

建立了高效液相色谱法测定猪、牛、羊、鸡的肝脏和肌肉组织中的辛硫磷残留量的检测方法。样品经乙酸乙酯提取,经C18固相萃取柱净化,80%乙腈-水溶液定容,以65%乙腈-水溶液为流动相,经高效液相色谱仪测定,外标法定量。结果表明：辛硫磷标准溶液在50~2 000μg/L范围内呈良好的线性关系,R2均为0.999 9,方法检出限为10μg/kg,最低定量限为20μg/kg,在20、50、100μg/kg添加水平上,辛硫磷的添加回收率为70%~120%,批内、批间RSD均小于20%。该残留检测技术具有简便、灵敏、定性定量准确、可靠等优点,满足动物性食品安全检测的要求。

A method based on high performance liquid chromatography（HPLC） has been developed for the determination of phoxim in animal derived food.The samples were extracted by ethylacetate,and cleaned up with C18 soild phase extraction（SPE） column,dissolved by 80% acetonitrile-water,and the final solution was confirmed by HPLC.Mobile phase in HPLC was 65% acetonitrile-water.The method was quantified by external standard method.The calibration curve was in good linearity between the peak area and the concentration of 50 to 2000 μg/L for phoxim with correlation coefficients R2=0.999 9.The detection limits of phoxim was 10 μg/kg,and the quantification limits was 20 μg/kg.The average recoveries from animal tissues at concentration range of 20,50,100 μg/kg range from 70% to 120%.The relative standard deviations of intra-and inter-batch were both less than 20%.The detection technology of phoxim residue was convenient,sensitive,accurate and reliable.It meets animal-derived food safety detection requirements of the relevant regulations.