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Determination of 4-Chloro-2-Methylphenoxyacetic Acid Residues in Wheat and Soil by Ultra-Performance Liquid Chromatography/Tandem Mass Spectrometry

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A rapid, highly sensitive, and selective method was developed for the identification and quantitation of the herbicide 4-chloro-2-methylphenoxyacetic acid (MCPA) in wheat plants, wheat grain, and soil by ultra-performance LC/MS/MS. MCPA was extracted from the sample (5 or 10 g) with acetonitrile, and an aliquot was taken for cleanup with primary secondary amine. Two precursor product ion transitions for MCPA were measured and evaluated to provide maximum confidence in the results. Average recoveries from wheat plants, wheat grain, and soil fortified at levels of 0.011.0 mg/kg ranged from 75.1 to 93.9, with RSDr values of 3.09.3 and RSDR values of 3.18.7. Coefficients of determination of R2 0.9994 were obtained for wheat and soil matrix calibration curves at MCPA levels of 0.015.0 g/mL. Under conditions of electrospray ionization in the negative-ion mode, the ion at m/z 141 was monitored for quantitation; the parent ion at m/z 199 was also measured. The LOD values for MCPA in wheat plants, wheat grain, and soil were determined to be 0.005, 0.004, and 0.004 mg/kg, respectively, and corresponding LOQ values were 0.02, 0.01, and 0.01 mg/kg. This method can be used to determinate MCPA residues in wheat products and soils.
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Document Type: Research Article

Affiliations: Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Beijing 100193, People's Republic of China.

Publication date: May 1, 2010

More about this publication?
  • The Journal of AOAC INTERNATIONAL publishes refereed papers and reviews in the fields of chemical, biological and toxicological analytical chemistry for the purpose of showcasing the most precise, accurate and sensitive methods for analysis of foods, food additives, supplements and contaminants, cosmetics, drugs, toxins, hazardous substances, pesticides, feeds, fertilizers and the environment available at that point in time. The scope of the Journal includes unpublished original research describing new analytical methods, techniques and applications; improved approaches to sampling, both in the field and the laboratory; better methods of preparing samples for analysis; collaborative studies substantiating the performance of a given method; statistical techniques for evaluating data. The Journal will also publish other articles of general interest to its audience, e.g., technical communications; cautionary notes; comments on techniques, apparatus, and reagents.
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