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

关键词:  高效液相色谱  辛硫磷  残留量  肌肉  肝脏

Key words:  high performance liquid chromatography  phoxim  residues  muscle  liver

摘要:

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50μg/L~2000μg/L范围内呈良好的线性关系，r 2均为0.9999，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。

Abstract:

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 2000μg/L for phoxim with correlation coefficients r 2=0.9999. The detection limits of phoxim was 10μg/kg, and the quantification limits was 20μg/kg. The average recoveries from animal tissues at concentration range of 20,50,100μg/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.