采用超高效液相色谱-串联质谱法同时检测水产品中孔雀石绿、结晶紫及其代谢物(隐色孔雀石绿、隐色结晶紫)。经匀浆处理的水产品样品,用乙腈提取,加入酸性氧化铝去除油脂,旋转蒸发器蒸干后,用甲酸-乙腈-水(0.1+10+89.9)溶液溶解,样品溶液用超高效液相色谱分离,电喷雾串联四极杆质谱进行检测。以氘代孔雀石绿、氘代隐色孔雀石绿为内标物。孔雀石绿、结晶紫及其代谢物的质量浓度均在5.0 μg·L-1以内与其峰面积呈线性关系,检出限(3S/N)在0.10~0.12 μg·kg-1之间。以空白水产品样品为基体进行回收试验,方法的回收率在90.2%~108.0%之间,相对标准偏差(n=6)在2.3%~7.6%之间。

UHPLC-MS/MS was applied to the determination of residual amounts of malachite green (MG), crystal violet (CV) and their metabolites, i.e., leuco-malachite green (LMG) and leuco-crystal violet (LCV), in aquatic products. The homogenized sample was extracted with acetonitrile and defatted by acidic aluminum oxide. The eluants were evaporated to dryness by rotary evaporator, and the residue was dissolved with HCOOH+CH3CN+H2O (0.1+10+89.9) mixture which was separated by UHPLC and analyzed by MS/MS. The malachite green D5 and leuco-malachite green D6 were used as internal standard. Linear relationships between values of peak area and mass concentration of the 4 compounds were found in the same range within 5.0 μg·L-1, with their detection limits (3S/N) in the range of 0.10-0.12 μg·kg-1. Using blank aquatic products as matrix, test for recovery was made by standard addition method, giving recovery in the range of 90.2%-108.0% with RSD′s (n=6) in the range of 2.3%-7.6%.