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    液相色谱-串联质谱法测定水产品中磺胺类及喹诺酮类药物残留量

    LC-MS/MS Determination of Residual Amounts of Sulfonamides and Quinolones in Aquatic Products

    • 摘要: 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5~200 μg·L-1,方法的测定下限(10S/N)在0.07~0.20 μg·kg-1之间。在1.0,4.0,20.0 μg·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。

       

      Abstract: 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 of n-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 5-200 μg·L-1, with lower limits of determination (10S/N) in the range of 0.07-0.20 μg·kg-1. Tests for recovery were made by standard addition method at 3 concentration levels of 1.0, 4.0, 20.0 μg·kg-1, giving values of recovery and RSD's (n=6) in the ranges of 80.3%-119% and 1.3%-12% respectively.

       

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