超高效液相色谱串联质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 UPLC-MS/MS

关键词:  超高效液相色谱串联质谱  辛硫磷  残留量  肌肉  肝脏

Key words:  UPLC-MS/MS  phoxim  residues  muscle  liver

摘要:

建立了超高效液相色谱串联质谱法（UPLC-MS/MS）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。样品用乙酸乙酯提取，提取液通过C18固相萃取柱净化，经超高效液相色谱串联质谱，外标法定量。结果表明：辛硫磷基质匹配标准溶液在0.01~1.00 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5 μg/kg，最低定量限为10 μg/kg。肝脏和肌肉组织在10、20、50 μg/kg添加水平上，辛硫磷的添加回收率为92.9%～102%，批内、批间相对标准偏差均小于10%。该残留检测方法具有简便、灵敏、定性定量准确、可靠等优点，能够满足动物性食品中辛硫磷残留的定性定量检测要求。

Abstract:

A method based on UPLC-MS/MS 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. The method was quantified by external standard method. The calibration curve was in good linearity between the peak area and the concentration of 0.01 to 1.00 μg/mL for phoxim with correlation coefficients R2>0.999. The detection limits of phoxim was 5 μg/kg, and the quantification limits was 10 μg/kg. The average recoveries from animal tissues at concentration range of 10, 20 and 50 μg/kg ranged from 92.9% to 102%. The relative standard deviations of intra-and inter-batch were both less than 10%. The detection technology of phoxim residue was convenient, sensitive, accurate and reliable. It meets animal-derived food detection requirements of the relevant regulations.