Multi-Residue Method for Pesticides Determination in Dried Hops by Liquid Chromatography Tandem Mass Spectrometry
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Published:2023-06-25
Issue:13
Volume:28
Page:4989
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ISSN:1420-3049
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Container-title:Molecules
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language:en
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Short-container-title:Molecules
Author:
Gruba Marcin1, Jóźwik Emilia1ORCID, Chmiel Mariusz1, Tyśkiewicz Katarzyna1ORCID, Konkol Marcin1, Watros Anna1, Skalicka-Woźniak Krystyna2ORCID, Woźniakowski Grzegorz3ORCID
Affiliation:
1. Łukasiewicz Research Network—New Chemical Syntheses Institute, Al. Tysiąclecia Państwa Polskiego 13a, 24-110 Puławy, Poland 2. Department of Natural Products Chemistry, Medical University of Lublin, ul. Chodźki 1, 20-093 Lublin, Poland 3. Department of Infectious and Invasive Diseases and Veterinary Administration, Institute of Veterinary Medicine, Faculty of Biological and Veterinary Sciences, Nicolaus Copernicus University in Toruń, Lwowska 1 Street, 87-100 Toruń, Poland
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.
Funder
THE MINISTRY OF EDUCATION NATIONAL SCIENCE CENTRE
Subject
Chemistry (miscellaneous),Analytical Chemistry,Organic Chemistry,Physical and Theoretical Chemistry,Molecular Medicine,Drug Discovery,Pharmaceutical Science
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