色谱

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱联用测定蜂王浆中的三种硝基咪唑类残留

丁涛1,徐锦忠1,沈崇钰1,蒋原1,陈惠兰1,吴斌1,赵增运1,李公海1,张婧1,刘飞2

  

  1. 1.National Honey Reference Laboratory, Animal, Plant and Food Inspection Center (APFIC)
    of Jiangsu Entry-exit Inspection and Quarantine Bureau, Nanjing 210001, China;
    2.Thermo Electron (Shanghai) Corporation, Shanghai 201206, China

  • 收稿日期:2006-02-27 修回日期:2006-04-30 出版日期:2006-07-30 发布日期:1986-12-25
  • 通讯作者: 丁涛

Determination of Three Nitroimidazole Residues in Royal Jelly by High Performance Liquid
Chromatography-Tandem Mass Spectrometry

DING Tao1, XU Jinzhong1, SHEN Chongyu1, JIANG Yuan1, CHEN Huilan1, WU Bin1, ZHAO Zengyun1, LI
Gonghai1, ZHANG Jing1, LIU Fei2

  

  1. 1.National Honey Reference Laboratory, Animal, Plant and Food Inspection Center (APFIC)
    of Jiangsu Entry-exit Inspection and Quarantine Bureau, Nanjing 210001, China;
    2.Thermo Electron (Shanghai) Corporation, Shanghai 201206, China

  • Received:2006-02-27 Revised:2006-04-30 Online:2006-07-30 Published:1986-12-25
  • Contact: DING Tao

摘要:

建立了高效液相色谱-串联质谱联用测定蜂王浆中甲硝唑(MTZ)、二甲硝唑(DMZ)和洛硝哒唑3(RNZ)种硝基咪唑类残
留的方法。使用氢氧化钠溶液溶解样品后,以乙酸乙酯液液萃取提取蜂王浆样品中的硝基咪唑类残留物。该法简便快捷,
适合大批量样品处理。采用氘代二甲硝唑作为内标和利用高选择性反应监测(H-RSM)技术,降低了基质干扰,增加了定量的
准确性。实验结果表明DMZ检测下限可以达到1.0 μg/kg,MTZ和RNZ检测下限可以达到0.5 μg/kg(S/N大于5);DMZ
定量下限可以达到2.0 μg/kg,MTZ和RNZ定量下限可以达到1.0 μg/kg(S/N大于10)。线性范围为2.0~200 μg/L,
添加回收率为96.6%~110.6%(内标校正),相对标准偏差(RSD)为2.1%~7.4%。

关键词: 串联质谱, 蜂王浆 , 高效液相色谱, 同位素内标, 硝基咪唑类化合物

Abstract:

A method for analysis of trace metronidazole (MTZ), dimetridazole (DMZ) and ronidazole
(RNZ) residues in royal jelly was developed by high performance liquid chromatography-tandem mass
spectrometry (HPLC-MS/MS). After samples were dissolved in sodium hydroxide solution to disassociate
target analytes from matrix, liquid-liquid extraction methods by ethyl acetate solvent were used.
Matrix effects were minimized and good quantitation results were obtained by using highly-selective
reaction monitoring (H-SRM) technology when deuterated dimetridazole (dimetridazole-D3) was selected
as internal standard. Limits of detection (LODs) were 1.0 μg/kg for DMZ, 0.5 μg/kg for MTZ and
RNZ (S/N>5). Limits of quantitation (LOQs) were 2.0 μg/kg for DMZ, 1.0 μg/kg for MTZ and RNZ
(S/N>10).The linear ranges were 2.0-200 μg/L for all target analytes. Recoveries and relative
standard deviations (RSDs) were in the ranges of 96.6%-110.6% and 2.1%-7.4%, respectively. This
method is suitable for statutory residue testing in the National Residue Surveillance Plan in China
and meets the requirement for export.

Key words:
deuterated internal standard,
nitroimidazole, royal jelly , tandem mass spectrometry (MS/MS), high performance liquid chromatography (HPLC)