采用超高效液相色谱-串联质谱法测定水产品中孔雀石绿和隐色孔雀石绿残留量。样品经乙腈提取,中性氧化铝固相小柱净化,C18色谱柱分离,电喷雾串联四极杆质谱进行检测。以氘代孔雀石绿和氘代隐色孔雀石绿为内标物。孔雀石绿和隐色孔雀石绿的线性范围均为0.25~20.0 μg·L-1,测定下限为0.50 μg·kg-1。以空白草鱼和大黄鱼空白样品为基体做加标回收试验,测得孔雀石绿的回收率在80.2%~105%之间,隐色孔雀石绿的回收率在85.1%~104%之间,相对标准偏差(n=6)均小于8%。

UHPLC-MS/MS was applied to the determination of residual amounts of malachite green and leuco-malachite green in aquatic products. The sample was extracted with acetonitrile and purified on neutral alumina solid phase column. The residue was taken up with 2 mL of mixture of acetonitrile and NH4OAc solution and separated by C18 chromatographic column and determined by MS/MS. The malachite green D5 and leuco-malachite green D6 were used as internal standards. Linearity ranges of malachite green and leuco-malachite green were found in the same range of 0.25-20.0 μg·L-1, with lower limits of determination of 0.50 μg·kg-1. Using blank samples of grass carp and large yellow croaker as matrixes, test for recovery was made by standard addition method, giving recovery of malachite green in the range of 80.2 %-105% and leuco-malachite green in the range of 85.1%-104%, with RSD′s (n=6) less than 8%.