Determination of selected herbicides in sugarcane-derived foods by graphene-oxide based disposable pipette extraction followed by liquid chromatography-tandem mass spectrometry

J Chromatogr A. 2023 Jan 4:1687:463690. doi: 10.1016/j.chroma.2022.463690. Epub 2022 Nov 28.

Abstract

Sugarcane is widely cultivated in Brazil. Although there are Maximum Residue Limits of pesticides determined for this plant, there is no legislation covering alimentary products from sugarcane. In this study, Disposable Pipette Tip Extraction (DPX) technique was evaluated as a sample preparation technique for simultaneous determination of eleven herbicides followed by LC-MS/MS analysis in three sugarcane-derived food matrices: juice, candy, and syrup. First, graphene oxide anchored to silica functionalized with octadecyl silane and endcapped was synthesized, which was evaluated as a sorbent in DPX. Then, after evaluating the parameters involved in DPX extraction, the method was validated following the ICH guide. As a result, the method showed acceptable linearity (r ≥ 0.99), limits of quantification (1.0 - 5.0 ng mL-1 for juice and 5.0 - 25.0 ng g - 1 for candy and syrup, varying according to the pesticide), precision, and accuracy within the limits of the literature, and recoveries ranging from 48 - 69% (juice), 34 - 89% (candy), and 28 - 76% (syrup). Finally, the developed method was successfully applied in actual samples of the three studied matrices.

Keywords: DPX. LC-MS/MS analysis; Disposable Pipette Extraction; Graphene oxide-based materials; Herbicides; Sugarcane.

MeSH terms

  • Chromatography, Liquid
  • Edible Grain
  • Graphite*
  • Herbicides*
  • Oxides
  • Pesticides*
  • Saccharum*
  • Solid Phase Extraction
  • Tandem Mass Spectrometry / methods

Substances

  • graphene oxide
  • Graphite
  • Herbicides
  • Pesticides
  • Oxides