应用高效液相色谱与串联质谱联用技术测定了鳗鱼中孔雀石绿(MG)、结晶紫(CV)及其代谢物(LMG,LCV)的残留量.样品用乙腈提取后,经脱脂、浓缩及净化处理,所得残渣用流动相混合液溶解后,通过Acquity UPLCTM BEH C18色谱柱分离,流出液供串联质谱测定,用氘代孔雀石绿及氘代无色孔雀石绿作内标参比定量.结果表明:对MG、LMG、CV、LCV四种化合物在0.1~10.0 μg·L-1范围内均呈线性关系,在0.5 μg·kg-1及2 μg·kg-1的标准加入水平下进行了回收试验,所得回收率在86.5%~91.8%之间,方法的检出限为0.1 μg·L-1(对MG及LMG)和0.5 μg·L-1(对CV及LCV),测定结果的相对标准偏差(n=7)≤7%.

High performance liquid chromatography in hyphenation with tendem mass spectrometry (HPLC-MS/MS) was applied to the determination of residual amounts of malachite green (MG),crystal violet (CV) and their leucobases (LMG and LCV).Sample of eel was extracted with acetonitrile,which was defatted,concentrated and purified.The residue obtained was dissolved in the mobile-phase solution and separated on the Acquity UPLCTM BEH C18 column.The eluate was used for tandem MS determination.Deuterium substituted MG and LMG were used as internal standards.Linear relationships were obtained in the ranges of 0.1~10 μg·L-1 for either of the MG,LMG,CV and LCV.Tests for recovery were made by addition of 0.5 μg·kg-1 and 2 μg·kg-1 of standards of MG,LMG,CV and LCV to blank flesh samples,and the results obtained were in the range of 86.5%-91.8%.Detection limits obtained were 0.1 μg·L-1 for MG and LMG,and 0.5 μg·L-1 for CV and LCV.Values of RSD′s (n=7) found for the determinations were ≤7%.