Direct Determination of 2,4-dichlorophenoxyacetic acid in Soybean and Corn by Liquid chromatography/tandem mass spectrometry

Authors

  • Narong Chamkasem Southeast Regional Laboratory, U.S. Food and Drug Administration, 60 Eighth Street, N.E., Atlanta, GA, 30309
  • Cynthia Morris Southeast Regional Laboratory, U.S. Food and Drug Administration, 60 Eighth Street, N.E., Atlanta, GA, 30309

DOI:

https://doi.org/10.21423/JRS-V04N02P009

Keywords:

2, 4-D, soybean, corn, LC-MS/MS, direct determination.

Abstract

A simple high-throughput liquid chromatography/tandem mass spectrometry (LC-MS/MS) method was developed for the determination of 2,4-dichlorophenoxy acetic acid (2,4-D) in soybean and corn using a reversed-phase with weak anion-exchange and cation-exchange mixed-mode Acclaim™ Trinity™ Q1 column. The method involved an alkaline hydrolysis with sodium hydroxide in order to convert all forms of 2,4-D into a salt form prior to extraction with acidified acetonitrile. The acetonitrile was salted out of the extract with sodium chloride and magnesium sulfate. The acetonitrile extract was diluted 1:1 with water and filtered before analysis by LC-MS/MS in a negative mode. Recoveries were evaluated at 10, 100, and 500 ng/g with seven replicates. Mean recovery ranged from 86 to 107% with relative standard deviation of less than 10%.  Matrix suppression was not observed in this procedure; therefore, no internal standard was needed. The method was used successfully for the determination of 2,4-D in soybean and corn samples containing incurred residue. The procedure proved to be quick, accurate, precise, sensitive, and selective.

https://doi.org/10.21423/jrs-v04n02p009 (DOI assigned 7/3/2019)

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Published

2016-05-05

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Scientific Articles