摘要
采用高效液相色谱法(HPLC)和四极杆飞行时间质谱法(TOFMS)联用技术测定了猪肉组织中20种兽药的残留量,包括16种磺胺类药物和4种β-受体激动剂类药物。猪肉样品(2.00g)用基质固相分散法处理后先后2次用乙腈-甲酸(99+1)混合液(每次20mL)振荡提取5min,离心分离后,取其上清液吹氮至近干,用甲醇-水(1+9)溶液1.0mL溶解浓缩物。经过滤后在所选仪器工作条件下进行HPLC-TOFMS分析。结果表明:20种目标化合物的线性范围均在0.2~400μg·L-1之间,其测定下限(10S/N)在0.4~15μg·kg-1之间。在3个浓度水平上用标准加入法进行回收试验,测得回收率在70.4%~109%之间,测定值的相对标准偏差(n=6)在6.7%~19%之间。
The method of HPLC in hyphenation with quadrupole-TOFMS was applied to the determination of residual amounts of 20veterinary drugs,including 16sulphonamides and 4β-recepter agonists.The pork sample(2.00g)was first treated by the method of matrix solid-phase dispersion and then extracted twice with 20mL(in each extraction)of a mixture of CH3CN-HCOOH(99+1).The supernatants were combined and evaporated to near dryness by N2-blowing,the concentrate was dissolved in 1.0mL of CH3OH-H2O(1+9)mixture,and used for HPLC-TOFMS analysis after filtration.Linearity ranges for the 20drugs were found same between 0.2-400μg·L-1,with lower limits of determination(10S/N)in the range of 0.4-15μg·kg-1.Test for recovery was made by standard addition method at 3concentration levels,giving values of recovery in the range of 70.4%-109% and values of RSD′s(n=6)ranged from 6.7%to 19%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2014年第6期702-707,共6页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
青岛市2013年"菜篮子"工程资助项目(青菜篮子[2013]1号)
