超高效液相色谱-串联质谱法测定水产品中孔雀石绿、结晶紫及其代谢物残留量

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5.0μg·L-1以内与其峰面积呈线性关系,检出限(3S/N)在0.10～0.12μg.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 Determination of Residual Amounts of Malachite Green, Crystal Violet and Their Metabolites in Aquatic Products

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%.