液相色谱-串联质谱法测定养殖鱼中痕量安眠酮的残留量

Determination of Trace Methaqualone Residues in Culture Fishes by Liquid Chromatography-Tandem Mass Spectrometry

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/z251.1/91.2为定量离子对,方法的定量限为0.2μg/kg(S/N≥10)。在0.2、0.5、1.0和20μg/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）=1∶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 μg/kg（S/N≥10）.Spike recoveries of four concentration levels（0.2,0.5,1.0 and 20 μg/kg） are in the range of 86.6%—95.9% with relative standard deviation of 2.26%—7.48%.