食品样品用乙腈提取,经弗洛里小柱净化后,用超高效液相色谱-串联质谱法测定其中9种抗凝血灭鼠剂的含量。色谱分离用甲醇和10 mmol·L-1乙酸铵溶液以不同体积比混合为流动相梯度洗脱,采用负离子模式电喷雾离子源在多反应监测模式下进行检测。噻鼠酮的检出限(3S/N)为0.38 μg·kg-1,其余8种灭鼠剂的检出限(3S/N)均为0.08 μg·kg-1。以空白食品样品为基体,加入3种浓度水平的灭鼠剂标准做回收试验,测得回收率在55.3%~118.1%之间,相对标准偏差(n=6)在2.2%~14.8%之间。

Foodstuff sample was extracted with acetonitrile, and the extract obtained was purified by passing through Florisil SPE column. The eluate obtained was determined and identified by HPLC-MS/MS. Mixtures of methanol and 10 mmol·L-1 ammonium acetate solution of various ratios were used as mobile phase in gradient elution and electrospray ionization source with negative ionization mode as well as multiple reaction monitoring mode were used in the MS/MS analysis. Values of detection limit (3S/N) found were 0.38 μg·kg-1 for difethialone and 0.08 μg·kg-1 for the remainder of 8. Tests for recovery were made by addition of standard rodenticide solutions at 3 different concentration levels to blank foodstuff sample matrixes, values of recovery found were in the range from 55.3% to 118.1%, with RSD′s (n=6) in the range from 2.2% to 14.8%.