UHPLC-MS/MS Determination of Residual Amounts of 9 Anticoagulant Rodenticides in Foodstuffs
标 签 超高效液相色谱-串联质谱法 抗凝血灭鼠剂 食品 UHPLC-MS/MS Anticoagulant rodenticides Foodstuffs
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%.
引用该论文: MI Jie-bo,CHEN Qi-yong,ZHAO Kong-xiang,WANG Yun-feng,CHANG Chun-yan,GE Bao-kun. UHPLC-MS/MS Determination of Residual Amounts of 9 Anticoagulant Rodenticides in Foodstuffs[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(3): 275～279
宓捷波,陈其勇,赵孔祥,王云凤,常春艳,葛宝坤. 超高效液相色谱-串联质谱法测定食品中9种抗凝血灭鼠剂的残留量[J]. 理化检验－化学分册, 2012, 48(3): 275～279