Determination of Underivatized Glyphosate Residues in Plant-Derived Food with Low Matrix Effect by Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry

A method was developed for the determination of glyphosate residues in plant-derived food using a two-step solid phase extraction (SPE) combined with mixed-mode liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with water. Then, the extracting solution was pretrea...

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Bibliographic Details
Published in:Food analytical methods 2016-10, Vol.9 (10), p.2856-2863
Main Authors: Ding, Junjie, Jin, Gehui, Jin, Gaowa, Shen, Aijin, Guo, Zhimou, Yu, Bing, Jiao, Yang, Yan, Jingyu, Liang, Xinmiao
Format: Article
Language:English
Subjects:
Analytical Chemistry
Anion exchanging
Cartridges
Chemistry
Chemistry and Materials Science
Chemistry/Food Science
Corn
Food
Food safety
Food Science
Liquid chromatography
Mass spectrometry
Matrices (mathematics)
Microbiology
Residues
Solid phases
Soybeans
Spectroscopy
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Summary:A method was developed for the determination of glyphosate residues in plant-derived food using a two-step solid phase extraction (SPE) combined with mixed-mode liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with water. Then, the extracting solution was pretreated by a C18 cartridge to remove protein and weak-polar interferences and further directly extracted using a strong anion exchange (SAX) cartridge to remove neutral and basic substances. The obtained glyphosate residues from the SPE were separated on a hydrophilic interaction/weak anion-exchange (HILIC/WAX) column and detected by mass spectrometry with negative electrospray ionization (ESI-) in multiple reaction monitoring (MRM) mode. This approach was evaluated by five different kinds of plant-derived food (soybean, corn, carrot, apple, and spicy cabbage) matrices in terms of matrix effect and recovery. Results showed that two-step SPE and mixed-mode chromatography separation provided the method with a very low matrix effect, and the spiked recoveries of glyphosate were satisfied in the range of 83.1 to 100.8 % at three spiked levels. The limit of quantification (LOQ) and detection (LOD) of the method in different matrices were 0.016–0.026 and 0.005–0.008 mg kg −1 , respectively. The procedure was validated and showed good accuracy and precision over a large linear range of 0.02–10 mg kg −1 .
ISSN:1936-9751
1936-976X
DOI:10.1007/s12161-016-0468-8