色谱

色谱 ›› 2013, Vol. 31 ›› Issue (5): 473-476.DOI: 10.3724/SP.J.1123.2012.11026

• 技术与应用 • 上一篇    下一篇

超高效液相色谱-串联质谱法同时快速筛查检测食品中的10种抗凝血类鼠药

朱峰, 刘华良*, 陈蓓, 荣维广, 马永建   

  1. 江苏省疾病预防控制中心, 江苏 南京 210009
  • 收稿日期:2012-11-28 修回日期:2013-01-24 出版日期:2013-05-28 发布日期:2013-05-16
  • 通讯作者: 刘华良,Tel:(025)83759366,E-mail:hejinshi@163.com.cn.
  • 基金资助:

    卫生部公益性行业科研专项项目(200902009);江苏省科技厅科技支撑计划项目(BE2010745);江苏省"十二五"科教兴卫工程项目(ZX201109).

Rapid simultaneous screening and detection of ten anticoagulant rodenticides in foods by ultra-high performance liquid chromatography-tandem mass spectrometry

ZHU Feng, LIU Hualiang*, CHEN Bei, RONG Weiguang, MA Yongjian   

  1. Jiangsu Provincial Center for Disease Prevention and Control, Nanjing 210009, China
  • Received:2012-11-28 Revised:2013-01-24 Online:2013-05-28 Published:2013-05-16

PDF

286

被引次数

13

摘要：

创建了一种利用超高效液相色谱-串联质谱同时快速筛查检测食品中10种抗凝血类鼠药的方法。试样用乙腈提取,QuEChERS净化,以5 mmol/L乙酸铵和乙腈为流动相进行梯度洗脱,经Poroshell 120 EC-C18柱(100 mm×2.1 mm, 2.7 μm;美国Agilent公司)分离,采用电喷雾电离(ESI)负离子质谱在多反应监测(MRM)模式下检测。10种鼠药均在5～500 μg/L范围内呈现良好的线性关系(r>0.99)。在辣椒酱、面粉、醋和酱油4种样品中,10种鼠药的加标回收率均在72.6%～112%范围内,相对标准偏差均不大于11.2%,检出限均在0.5～4.5 μg/kg范围内。本方法快速、简便、灵敏、重现性好,能满足由此10种抗凝血类鼠药引发的突发性公共卫生安全事件的快速筛查与检测要求。

关键词: 超高效液相色谱-串联质谱, 抗凝血类鼠药, 食品

Abstract:

A rapid method for the simultaneous screening and detection of ten anticoagulant rodenticides in foods was developed by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). After the extraction by acetonitrile and clean-up by QuEChERS, the extract was separated on a Poroshell 120 EC-C18 column (100 mm×2.1 mm, 2.7 μm) with the gradient elution of 5 mmol/L ammonium acetate and acetonitrile. The detection was carried out by UPLC-MS/MS using a negative electrospray ionization interface in multiple reaction monitoring (MRM) mode. The ten anticoagulant rodenticides showed a good linear relationship (r>0.99) in the range of 5-500 μg/L. In the four samples of chili sauce, flour, vinegar and soy sauce, the spiked recoveries were in the range of 72.6%-112%, and the relative standard deviations (RSD) were all not more than 11.2%. The limits of detection (LOD) were all in the range of 0.5-4.5 μg/kg. This method is rapid, simple, sensitive, accurate and of good specificity for the satisfactory rapid screening and detection of the ten anticoagulant rodenticides in the sudden public health security events.

Key words: anticoagulant rodenticides, foods, ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

中图分类号: