谱尼测试-论QuEChERS-UPLC-MSMS测定果蔬中四种残留抗凝血杀鼠剂.pdf

QuEChERS-UPLC-MS/MS 测定果蔬中四种残留抗凝血杀鼠剂 谱尼测试集团股份有限公司 摘 要： 采用QuEChERS 前处理方法，结合超高效液相色谱- 串联质谱（UPLC-MS/MS ）技术建立了测定 蔬菜、水果中灭鼠灵、杀鼠迷、溴鼠灵、氟鼠酮等四种抗凝血杀鼠剂残留量的方法。于Waters DisQue 提取管中，粉碎匀浆的样品由含冰醋酸体积分数1%的乙腈提取并净化后，UPLC BEH C18 液相色谱柱 - 分离，流动相用甲醇和含5 mmol/L 乙酸铵和体积分数甲酸0.1 ％的水溶液梯度洗脱，ESI-[M-H] 电离， 多反应监测模式，外标法定量。试验了往DisQue 净化管中分别补加PSA （氨基吸附剂）和GCB （石 墨化碳黑）填料净化对回收率的影响, 结果显示5mg 的GCB 可以取得，满意的效果。方法中灭鼠灵 和杀鼠迷的在0.5~100 µg/L 线性相关, 方法检出限(LOD)为0.25 µg/kg，溴鼠灵和氟鼠酮在2~250 µg/L 线性相关，LOD 为1.0 µg/kg。在低、中、高三个添加水平的加标回收率为86%～128%，相对标准偏 差(RSD%) 2.4%～16%。 关键词：抗凝血杀鼠剂；果蔬残留；灭鼠灵；杀鼠迷；溴鼠灵；氟鼠酮 中图分类号：TS207.3 文献标识码：A 文章编号： Determination of Four Anticoagulant Rodenticides Residues in Vegetables and Fruits Using QuEChERS-UPLC-MS/MS SONG Wei, YANG Bai-chong, ZHAO Yong-biao, SONG Gui-xue* （Pony Testing Co. Ltd., Beijing 10008, China ） Abstract ：Using QuEChERS pretretment, a method was established to detect warfarin, coumatetralyl, brodifacoum and flocoumafen in vegetables and fruits with ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Grounded and homogenized samples were extracted by mixed with acetonnitrile containing 1% (v/v) glacial acetic acid in Waters DisQue tubes and cleaned up. Components in the supernatant were separated by an UPLC BEH C18 column and eluted by methanol and 5 mmol/L ammonium acetate and 0.1% (v/v) formic acid solution with gradient elution. Analysis was accomplished by ESI-[M-H]- with multiple reaction monitor (MRM) mode and external standard quatification. In order to eliminate matrix effect, DisQue purification tubes with additiona