建立了液相色谱-串联质谱测定养殖鱼类产品中痕量安眠酮(MTQ)残留量的方法.采用正己烷提取样品中残留的安眠酮,经硅胶柱净化、V(乙醚):V(正己烷)=1∶1的混合溶液洗脱后,以0.1％V(甲酸):V(甲醇)=1∶1的混合溶液为流动相、C18色谱柱分离,正离子模式进行质谱定量分析,MTQ-D7同位素标记物作为内标,用内标法定量.以m/z 251.1/91.2为定量离子对,方法的定量限为0.2 μg/kg(S/N≥10).在0.2、0.5、1.0和20 μg/kg 4个添加水平下,方法的平均回收率为86.6％～95.9％,相对标准偏差为2.26％～7.48％.%A method of liquid chromatography-tandem mass spectrometry was developed for the determination of trace methaqualone(MTQ) residues in culture fish samples. The samples were extracted by n-hexane, purified on Silica column, eluted by V(ethyl ether): V(hexan) = l : 1 and separated by liquid chromatography on C18 column with mobile phase of 0. 1 % formic acid in methanol. MTQ-D7 was used as internal standard, the quantification was performed with internal standard method. An ion pair of m/z 251. 1/91. 2 was used for the quantitative analysis of MTQ by MS. The limit of determination is 0. 2 fig/kg (S/N≥ 10). Spike recoveries of four concentration levels (0. 2, 0. 5, 1.0 and 20 fig/kg) are in therange of 86. 6%-95. 9% with relative standard deviation of 2. 26%-7. 48%.
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