采用超高效液相色谱(UHPLC)与串联质谱(MS/MS)联用对水产品中残留量的孔雀石绿(MG)及无色孔雀石绿(LMG)进行了快速检测.经均匀化处理的试样用乙腈在pH 4.5的乙酸盐缓冲介质中萃取使MG及LMG萃入有机相，所得萃取液用液-液分配，先后用酸性氧化铝及氯化钠和酸性氧化铝及无水硫酸钠进行分离及净化.上层清液经0.2 μm滤膜过滤后供UHPLC-MS/MS分析,采用电喷雾离子化(ESI+)及多反应监测模式进行测定,用D5-MG及D6-LMG内标法进行定量.在优化的试验条件下，使质谱分析中的基体效应得到合理降低.方法的测定下限(S/N=10)，MG为0.19 μg·kg-1,LMG为0.10 μg·kg-1,在0.5~5.0 μg·kg-1浓度范围内作标准加入法,方法的回收率在89.4%~110%范围内.相对标准偏差(n=6)值在5.9%~9.8%.

Residual amounts of malachite green (MG) and leuco malachite green (LMG) in aquatic products were determined by ultra-high performance liquid chromatography (UHPLC) hyphenated with tandem mass spectrometry (MS/MS).The compounds,MG and LMG,were extracted from the homogenized tissue sample with acetonitrile in an acetate buffer medium of pH 4.5,separated and purified by liquid-liquid partition and acidic alumina and sodium chloride,as well as acidic alumina and anhydrous sodium sulfate in succession.The clear supernatant liquid after fitration with 0.2 μm filtering membrane was ready for UHPLC-MS/MS analysis.Determinations were performed by using electrospray ionization (ESI+) and multi-reaction monitoring (MRM) modes.Internal standards of D5-MG and D6-LMG were used in the quantification.Under optimized conditions of sample pretreatment and operation of instruments,matrix effect on the MS determination was reduced rationally.Determination (S/N=10) for MG and LMG were found to be 0.19 and 0.10 μg·kg-1 respectively.Tests for recovery were made by addition of standards in the concentration range of 0.5 to 5.0 μg·kg-1,and results obtained were ranged from 89.4% to 110%.Values of RSD′s (n=6) were found in the range of 5.9%-9.8%.