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(2.00 g)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20 mL)振荡提取5 min,离心分离后,取其上清液吹氮至近干,用甲醇水(1+9)溶液1.0 mL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0.2~400 μg·L-1之间,其测定下限(10S/N)在0.4~15 μg·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 20 veterinary drugs, including 16 sulphonamides and 4 βrecepter agonists. The pork sample (2.00 g) was first treated by the method of matrix solidphase dispersion and then extracted twice with 20 mL (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 1.0 mL of CH3OHH2O (1+9) mixture, and used for HPLCTOFMS analysis after filtration. Linearity ranges for the 20 drugs were found same between 0.2-400 μg·L-1, with lower limits of determination (10S/N) in the range of 0.4-15 μg·kg-1. Test for recovery was made by standard addition method at 3 concentration 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%.