水产品样品(5.00 g)经乙腈-甲酸(99+1)混合液20 mL提取,无水乙醇除水,浓缩并加正己烷2 mL脱脂.所得溶液进行液相色谱分离.以ACQUITY UPLC BEH HILIC色谱柱为分离柱,以不同体积比的甲醇和0.1%(体积分数)甲酸溶液的混合液为流动相进行梯度洗脱.质谱分析中,采用电喷雾正离子源多反应监测模式检测.采用内标法定量.所涉11种药物的线性范围均为5~200μg·L-1,方法的测定下限(10S/N)在0.07~0.20μg·kg-1之间.在1.0,4.0,20.0μg·kg-1等3个浓度水平进行加标回收试验,回收率在80.3%~119%之间,测定值的相对标准偏差(n=6)在1.3%~12%之间.%The sample of aquatic products (5 .00 g)was extracted with 20 mL of a mixture of acetonitrile and formic acid (99+1 ).The extract was dehydrated with absolute ethanol.The extract was then concentrated and 2 mL ofn-hexane was added to remove fat.LC separation was performed by using ACQUITY UPLC BEH HILIC chromatographic column as stationary phase,and mixtures of methanol and 0 .1% (φ)formic acid solution with various ratios as mobile phase in gradient elution.ESI+ and multi-reaction-monitoring were adopted in MS/MS. Internal standard method was used for quantification.Linearity ranges of the 11 drugs were found in the same range of 5-200μg·L-1 ,with lower limits of determination (10S/N)in the range of 0.07-0.20μg·kg-1 .Tests for recovery were made by standard addition method at 3 concentration levels of 1.0,4.0,20.0μg·kg-1 ,giving values of recovery and RSD′s (n= 6)in the ranges of 80.3%-119%and 1.3%-12%respectively.
展开▼
