提出了高效液相色谱-串联质谱法测定动物组织中尼卡巴嗪残留量的方法.样品经N,N-二甲基甲酰胺-乙腈 (10+90)混合溶液提取,饱和的正己烷脱脂后,离心分离取下层溶液过Waters Sunfire C18色谱柱(150 mm×2.1 mm,3.5 μm)分离,串联质谱法进行测定,同位素内标法定量.残留尼卡巴嗪的标识物4,4′-二硝基碳酰替苯胺(DNC)的质量浓度在0.010~0.200 mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)为30 ng·g-1,测定下限(10S/N)为50 ng·g-1.以3类动物组织样品为基体,加入3种不同浓度水平的DNC标准溶液作回收试验,测得回收率分别在72.2%~88.6%之间,相对标准偏差(n=6)在1.63%~12.1%之间.

It was reported that residual amount of nicarbazin in animal tissue was determined by HPLC-MS/MS.Samples were extracted with a mixed solution of N,N-dimethylformamide and acetonitrile (10+90),and defatted with saturated n-hexane.After centrifugation,an aliquot of the lower layer solution was taken for separation by passing through Waters Sunfire C18 column (150 mm×2.1 mm,3.5 μm),and the content of labelled compound 4,4′-dinitro-carbanilide (DNC) for residual nicarbazin was determined by MS/MS with isotopic internal standard.Linear relationship between values of peak area and mass concentration of DNC was kept in the range of 0.010-0.200 mg·L-1,with values of detection limit (3S/N) of 30 ng·g-1 and lower limit of determination (10S/N) of 50 ng·g-1.Tests for recovery were made by addition of standard DNC at 3 different concentration levels to 3 kinds of animal tissues as matrixes,values of recovery found were in the range of 72.2%-88.6%,with values of RSD′s (n=6) in the range from 1.63% to 12.1%.