稻米中11种农药残留QuEChERS/UPLC-MS/MS测定方法的研究

Research of detecting eleven kinds of pesticide residues in rice QuEChERS/UPLC-MS/MS

建立和优化了QuEChERS/超高效液相色谱-质谱联用(UPLC-MS/MS)检测稻米中多农药残留的方法。采取QuECHERS前处理方法,UPLC-MS/MS同时检测11种农药残留。11种农药的3水平添加回收率在70.9%~92.7%之间,日间精密度和日内精密度均小于10%,检出限(LOD)为0.002~0.14μg/kg,定量限(LOQ)在0.01~0.4μg/kg之间。外标法定量,11种农药在线性范围内具有良好的线性关系,相关系数均大于0.999。QuEChERS前处理方法简单、上机检测时间短、灵敏度高、精密度和准确度较好,能够较好地满足稻米中常见农药残留的检测。

A QuEChERS/ultra high performance liquid chromatography-mass spectrometry(UPLC-MS/MS)method was established and optimized for the determination of multiple pesticide residues in rice.QuECHERS pretreatment method was adopted and UPLC-MS/MS was used to detect 11 pesticide residues simultaneously.The 3-level recoveries of the 11 pesticides ranged from 70.9%to 92.7%,and the inter-day and intra-day precision were all less than 10%.The detection limit(LOD)and quantification limit(LOQ)of the 11 pesticides ranged from 0.002 to 0.14μg/kg and from 0.01 to 0.4μg/kg.By external standard method,11 pesticides had good linear relationship in the linear range,and the correlation coefficient was greater than 0.999.The QuEChERS pretreatment method was simple,with short detection time on the computer,high sensitivity,good precision and accuracy,which could better meet the detection of common pesticide residue in rice.