采用超高效液相色谱-串联质谱法测定水产品中孔雀石绿及其代谢物的残留量。样品经盐酸羟胺、对甲苯磺酸、乙酸铵的混合液作为提取剂均质提取,乙腈萃取,并通过-18 ℃冷冻离心分层。以ACQUITY UPLC BEH C18色谱柱分离,用乙腈与5 mmol·L-1乙酸铵溶液(75+25)的混合液洗脱,采用正离子模式监测。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1.0~20.0 μg·L-1,检出限(3S/N)依次为0.05,0.06 μg·kg-1。在1.0,2.0,5.0 μg·kg-1等3个浓度水平进行加标回收试验,回收率在90.2%~106%之间,测定值的相对标准偏差(n=6)在2.1%~11%之间。

UHPLC-MS/MS was applied to the determination of residual amounts of malachite green and its metabolite in aquatic product. The sample was treated by homogeneous extraction with extracting agent of mixed solution of hydroxylamine hydrochloride, toluene-p-sulfonic acid and ammonium acetate, and then extracted with acetonitrile. Phase-separation was attained by freezing centrifugation at -18 ℃. ACQUITY UPLC BEH C18 column was used as stationary phase and a mixture of acetonitrile and 5 mmol·L-1 ammonium acetate (75+25) was used as mobile phase in chromatographic separation. Positive electrospray ionization was used in the detection. 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 same between 1.0-20.0 μg·L-1 with detection limits (3S/N) of 0.05, 0.06 μg·kg-1 respectively. Tests for recovery were made by standard addition method at 3 concentration levels of 1.0, 2.0, 5.0 μg·kg-1, giving values of recovery and RSD′s (n=6) in the ranges of 90.2%-106% and 2.1%-11% respectively.