超高效液相色谱-串联质谱法快速检测菜豆及土壤中的灭蝇胺残留

徐军; 张盈; 董丰收; 刘新刚; 郭紫兰; 郑永权

超高效液相色谱-串联质谱法快速检测菜豆及土壤中的灭蝇胺残留

1.
中国农业科学院植物保护研究所,北京 100193
2.
湖南农业大学生物安全科学技术学院,长沙 410128

基金项目:

国家自然科学基金资助项目(31171879;31000863).

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出版历程
- 收稿日期: 2012-08-22
- 修回日期: 2012-09-27

Determination of cyromazine residues in common bean and soil using ultraperformance liquid chromatography-tandem mass spectrometry

1.
Institute of Plant Protection, Chinese Academy of Agricultural Science, Beijing 100193, China
2.
College of Bio-Safety Science & Technology, Hunan Agricultural University, Changsha 410128, China

摘要

摘要: 建立了采用超高效液相色谱-串联质谱仪(UPLC-MS/MS)快速检测分析菜豆及其土壤中灭蝇胺残留的方法。样品经5 mmol/L的乙酸铵-乙腈溶液[V(乙酸铵):V(乙腈)=1:4]提取、定容,N-丙基乙二胺(PSA)净化后用UPLC-MS/MS在正离子模式下以多反应监测扫描方式进行测定,外标法定量。结果表明:在0.05～1 mg/kg添加水平范围内,灭蝇胺在菜豆和土壤中的平均回收率为80.1%～95.2%,相对标准偏差(RSD)为1.9%～9.1%,检出限(LOD)为3.8～5.9 μg/kg,定量限(LOQ)为50 μg/kg。该方法操作简单、灵敏度高、定量准确且测定浓度范围宽,适用于菜豆及土壤中灭蝇胺的残留分析。
- 超高效液相色谱-串联质谱 /
- 灭蝇胺 /
- 残留 /
- 菜豆 /
- 土壤
Abstract: A rapid method for determination of cyromazine residues in common bean(Phaseolus vulgaris) and soil was established based on ultraperformance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The sample was extracted with 5 mmol/L solution of ammonium acetate and acetonitrile [V(acetate):V(acetonitrile)=1:4] and then purified by primary secondary amine(PSA).The cyromazine residues were analyzed by UPLC-MS/MS under multiple reaction monitoring mode and quantified with external standards.Average recoveries of cyromazine in common bean and soil at three levels(0.05,0.5 and 1 mg/kg) ranged from 80.1% to 95.2% with relative standard deviations from 1.9% to 9.1%.Limits of detection of cyromazine were 3.8-5.9 μg/kg,while limits of quantification were 50 μg/kg.The method is simple and suitable for the routine and confirmation analysis of cyromazine residue.
- ultraperformance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) /
- cyromazine /
- residue /
- common bean(Phaseolus vulgaris) /
- soil

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参考文献(12)

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