Determination of Glufosinate Residue in Vegetables and Fruits by Liquid Chromatography-Tandem Mass Spectrometry with Purification of Solid Phase Extraction
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Determination of Glufosinate Residue in Vegetables and Fruits by Liquid Chromatography-Tandem Mass Spectrometry with Purification of Solid Phase Extraction
Vol. 34, Issue 9, Pages: 993-998(2015)
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上海出入境检验检疫局
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Determination of Glufosinate Residue in Vegetables and Fruits by Liquid Chromatography-Tandem Mass Spectrometry with Purification of Solid Phase Extraction. [J]. 34(9):993-998(2015)
DOI:
Determination of Glufosinate Residue in Vegetables and Fruits by Liquid Chromatography-Tandem Mass Spectrometry with Purification of Solid Phase Extraction. [J]. 34(9):993-998(2015)DOI:
Determination of Glufosinate Residue in Vegetables and Fruits by Liquid Chromatography-Tandem Mass Spectrometry with Purification of Solid Phase Extraction
A liquid chromatography-tandem mass spectrometric(LC-MS/MS) method was established for the determination of glufosinate-ammonium residue in vegetables and fruits.The samples spiked with d3-glufosinate,the internal standard,were extracted with water,defatted with dichloromethane,and cleaned up using a strong cation exchange column,then derived with 9-fluorenylmethylchloroformate(FMOC-Cl) overnight.The separation of the target compound was performed on a C18 column(4.6 mm×50 mm,1.8 μm) using 5 mmol/L ammonium acetate(containing 0.1% formic acid)-acetonitrile(containing 0.1% formic acid) as mobile phase.The identification and quantitation of glufosinate were performed by MS/MS in positive electrospray ionization(ESI+) and multiple reaction monitoring(MRM) mode.The quantitative analysis was carried out by the internal standard method.The calibration curve showed a good linearity in the range of 0-200 μg/L with a correlation coefficient greater than 0.995.The limit of detection(LOD) and the limit of quantitation(LOQ) of this method were 10 μg/kg and 20 μg/kg,respectively.The average recoveries of glufosinate in foods at three spiked levels of 20,200,500 μg/kg were in the range of 80.8%-102.2% with relative standard deviations(RSDs) of 1.8%-7.9%.The application of internal standard effectively reduced the influence of matrix effects.The results of validation tests indicated that the method was sensitive and accurate,and was suitable for the monitoring of glufosinate residue in vegetables and fruits.
关键词
草铵膦残留固相萃取液相色谱-串联质谱
Keywords
glufosinateresiduesolid phase extractionliquid chromatography-tandem mass spectrometry
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Related Author
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Related Institution
College of Horticulture and Landscape,Tianjin Agricultural University
Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables;Key Laboratory of Quality and Safety Control for Subtropical Fruit and Vegetable,Ministry of Agriculture and Rural Affairs;Analysis and Test Center,Chinese Academy of Tropical Agricultural Sciences
Tea Research Institute,Chinese Academy of Agricultural Sciences
Key Laboratory of Tropical Fruits and Vegetables Quality and Safety for State Market Regulation;Hainan Institute for Food Control
Key Laboratory of Pesticide Environmental Assessment and Pollution Control,Ministry of Environmental Protection,Nanjing Institute of Environmental Sciences,Ministry of Ecology and Environment of the People’s Republic of China