Multi-Residue Method for Pesticides Determination in Dried Hops by Liquid Chromatography Tandem Mass Spectrometry
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, C<sub>18</sub>, GCB, Z-...
| Main Authors: | , , , , , , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
MDPI AG
2023-06-01
|
| Series: | Molecules |
| Subjects: | |
| Online Access: | https://www.mdpi.com/1420-3049/28/13/4989 |
| _version_ | 1797591192964169728 |
|---|---|
| author | Marcin Gruba Emilia Jóźwik Mariusz Chmiel Katarzyna Tyśkiewicz Marcin Konkol Anna Watros Krystyna Skalicka-Woźniak Grzegorz Woźniakowski |
| author_facet | Marcin Gruba Emilia Jóźwik Mariusz Chmiel Katarzyna Tyśkiewicz Marcin Konkol Anna Watros Krystyna Skalicka-Woźniak Grzegorz Woźniakowski |
| author_sort | Marcin Gruba |
| collection | DOAJ |
| description | 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, C<sub>18</sub>, 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 (RSD<sub>r</sub>) 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. |
| first_indexed | 2024-03-11T01:33:59Z |
| format | Article |
| id | doaj.art-36e25c7bc5634e578aeed8a011d000da |
| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-11T01:33:59Z |
| publishDate | 2023-06-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-36e25c7bc5634e578aeed8a011d000da2023-11-18T17:06:33ZengMDPI AGMolecules1420-30492023-06-012813498910.3390/molecules28134989Multi-Residue Method for Pesticides Determination in Dried Hops by Liquid Chromatography Tandem Mass SpectrometryMarcin Gruba0Emilia Jóźwik1Mariusz Chmiel2Katarzyna Tyśkiewicz3Marcin Konkol4Anna Watros5Krystyna Skalicka-Woźniak6Grzegorz Woźniakowski7Łukasiewicz Research Network—New Chemical Syntheses Institute, Al. Tysiąclecia Państwa Polskiego 13a, 24-110 Puławy, PolandŁukasiewicz Research Network—New Chemical Syntheses Institute, Al. Tysiąclecia Państwa Polskiego 13a, 24-110 Puławy, PolandŁukasiewicz Research Network—New Chemical Syntheses Institute, Al. Tysiąclecia Państwa Polskiego 13a, 24-110 Puławy, PolandŁukasiewicz Research Network—New Chemical Syntheses Institute, Al. Tysiąclecia Państwa Polskiego 13a, 24-110 Puławy, PolandŁukasiewicz Research Network—New Chemical Syntheses Institute, Al. Tysiąclecia Państwa Polskiego 13a, 24-110 Puławy, PolandŁukasiewicz Research Network—New Chemical Syntheses Institute, Al. Tysiąclecia Państwa Polskiego 13a, 24-110 Puławy, PolandDepartment of Natural Products Chemistry, Medical University of Lublin, ul. Chodźki 1, 20-093 Lublin, PolandDepartment 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, PolandIn 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, C<sub>18</sub>, 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 (RSD<sub>r</sub>) 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.https://www.mdpi.com/1420-3049/28/13/4989dried hopshop conespesticide residuesQuEChERSLC-MS/MS |
| spellingShingle | Marcin Gruba Emilia Jóźwik Mariusz Chmiel Katarzyna Tyśkiewicz Marcin Konkol Anna Watros Krystyna Skalicka-Woźniak Grzegorz Woźniakowski Multi-Residue Method for Pesticides Determination in Dried Hops by Liquid Chromatography Tandem Mass Spectrometry Molecules dried hops hop cones pesticide residues QuEChERS LC-MS/MS |
| title | Multi-Residue Method for Pesticides Determination in Dried Hops by Liquid Chromatography Tandem Mass Spectrometry |
| title_full | Multi-Residue Method for Pesticides Determination in Dried Hops by Liquid Chromatography Tandem Mass Spectrometry |
| title_fullStr | Multi-Residue Method for Pesticides Determination in Dried Hops by Liquid Chromatography Tandem Mass Spectrometry |
| title_full_unstemmed | Multi-Residue Method for Pesticides Determination in Dried Hops by Liquid Chromatography Tandem Mass Spectrometry |
| title_short | Multi-Residue Method for Pesticides Determination in Dried Hops by Liquid Chromatography Tandem Mass Spectrometry |
| title_sort | multi residue method for pesticides determination in dried hops by liquid chromatography tandem mass spectrometry |
| topic | dried hops hop cones pesticide residues QuEChERS LC-MS/MS |
| url | https://www.mdpi.com/1420-3049/28/13/4989 |
| work_keys_str_mv | AT marcingruba multiresiduemethodforpesticidesdeterminationindriedhopsbyliquidchromatographytandemmassspectrometry AT emiliajozwik multiresiduemethodforpesticidesdeterminationindriedhopsbyliquidchromatographytandemmassspectrometry AT mariuszchmiel multiresiduemethodforpesticidesdeterminationindriedhopsbyliquidchromatographytandemmassspectrometry AT katarzynatyskiewicz multiresiduemethodforpesticidesdeterminationindriedhopsbyliquidchromatographytandemmassspectrometry AT marcinkonkol multiresiduemethodforpesticidesdeterminationindriedhopsbyliquidchromatographytandemmassspectrometry AT annawatros multiresiduemethodforpesticidesdeterminationindriedhopsbyliquidchromatographytandemmassspectrometry AT krystynaskalickawozniak multiresiduemethodforpesticidesdeterminationindriedhopsbyliquidchromatographytandemmassspectrometry AT grzegorzwozniakowski multiresiduemethodforpesticidesdeterminationindriedhopsbyliquidchromatographytandemmassspectrometry |