王艺纯,郭美玲,唐秋竹,李秀芬,徐飞.液质联用法测定人参中氟啶胺的残留[J].中国药事,2017,(5):550-554 |
液质联用法测定人参中氟啶胺的残留 |
Determination of the Residue of Fluazinam in Ginseng by Liquid Chromatography-Tandem Mass Spectrometry |
投稿时间:2016-11-14 |
DOI:10.16153/j.1002-7777.2017.05.015 |
中文关键词: 氟啶胺 人参 农药残留 液质联用 含量测定 |
英文关键词: fluazinam ginseng pesticide residue LC-MS/MS content determination |
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中文摘要: |
目的:建立高效液相色谱-电喷雾串联四级杆质谱法测定人参中氟啶胺的残留量。方法:采用固相萃取技术进行样品前处理,采用Waters BEH C18色谱柱(2.1 mm×150 mm,1.7 μm),以乙腈-5 mM乙酸铵为流动相梯度洗脱,电喷雾离子源负离子模式多反应监测(MRM)模式定性分析,采用外标曲线法对人参中氟啶胺的残留量进行检测。结果:氟啶胺浓度在0.0015~0.4 μg·L-1具有良好的线性关系,r=1.0000;加样回收率符合要求;方法的检出限(信噪比S/N=3)为1.1 μg·kg-1。结论:本方法易于操作,结果准确,重现性良好,可用于人参中氟啶胺残留量的测定。 |
英文摘要: |
Objective: To establish the quality standard of liquid chromatography-tandem mass spectrometry (LC-MS/MS) for the determination of residue of fluazinam in ginseng. Methods: Samples were purified with SPE column and residue of fluazinam was determined by LC-MS/MS under multiple reaction-monitoring negative ionization mode (MRM) using external calibration curve with Waters BEH C18 column (2.1 mm×150 mm, 1.7 μm) and the mobile phase of acetonitrile-ammonium acetate gradient elution for separation with HPLC. Results: The linear range of concentrations of fluazinam was 0.0015~0.4 μg·L-1 (r=1.0000) with a good linear relationship. The recovery rates were satisfactory and the detection limit (S/N=3) was 1.1 μg·kg-1. Conclusion: The method is simple, rapid, precise, and reproducible, which can be used for the determination of residue of fluazinam in ginseng. |
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