Multi-Residue Method for Pesticides Determination in Dried Hops by Liquid Chromatography Tandem Mass Spectrometry

Molecules. 2023 Jun 25;28(13):4989. doi: 10.3390/molecules28134989.

Abstract

In this study a multi-residue determination method for 36 pesticides in dried hops was reported. The sample preparation procedure was based on the acetate buffered QuEChERS method. A few mixtures of dispersive solid phase extraction (dSPE) sorbents consisting PSA, C18, GCB, Z-Sep and Z-Sep+ were investigated to clean-up the supernatant and minimize matrix co-extractives. The degree of clean-up was assessed by gravimetric measurements, which showed the best results for mixtures containing the Z-Sep+ sorbent. This is the first study to apply Z-Sep+ sorbent for hops material and the first to improve the method for pesticide residues determination in hops. Samples were analysed using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) and the procedure was validated according to the SANTE/11813/2017 document at four concentration levels: 0.02, 0.05, 0.1 and 1 mg/kg. The limits of quantification (LOQ) were in the range of 0.02-0.1 mg/kg. For all active substances, the trueness (recovery) ranged from 70 to 120% and the precision (RSDr) value was <20%. Specificity, linearity and matrix effect were also evaluated. The validated method was applied to the analysis of 15 real dried hop samples and the relevant data on detected residues were included.

Keywords: LC-MS/MS; QuEChERS; dried hops; hop cones; pesticide residues.

MeSH terms

  • Chromatography, Liquid / methods
  • Humulus*
  • Pesticide Residues* / analysis
  • Pesticides* / analysis
  • Solid Phase Extraction / methods
  • Tandem Mass Spectrometry / methods

Substances

  • Pesticides
  • Pesticide Residues