The aim of this study was the evaluation of compatibility of mixtures of pesticides with white wine matrix in order to establish that all the criteria for a candidate reference material were met (homogeneity, stability, definition of certified property values and related uncertainties). The matrix selected for this assay was a pesticide free white wine (i.e. containing selected pesticides at levels lower than the relevant limit of detection, L.O.D.). The spiking mixtures to be included in the matrix were composed by a selection of pesticides usually found in viticulture, belonging to different chemical classes and characterized by specific mode of action. According to CIPAC Method MT 46, the matrices spiked with pesticide mixtures were stressed at 54°C for 14 days in order to investigate on the achievable long-term stability. Pesticide mixtures were analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS) evaluating the intrinsic amenability to this analytical technique for every single compound and taking into account data of annex B of European EN 15662:2009 "Foods of plant origin - Determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by dispersive SPE - QuEChERS-method". White wine is a high water content matrix (80-100%) and contains a variable amount of carbohydrates and organic acids. Therefore extraction and clean-up were performed according to QuEChERS procedure, according to annex C of EN 15662:2009. The quantitative determination of pesticides in the wine matrix mixture was accomplished by LC-MS/MS and LC-HRMS based in Orbitrap technology. Tuning of instrumental parameters for the multiresidue method, either LC-MS/MS and LC-HRMS settings, was performed by direct infusion of every single pesticide. Data were acquired in Selected Reaction Monitoring mode for LC-MS/MS and HR Full Scan mode for LC-HRMS. In order to fulfill the requirements specified in the document SANCO 10684/2013 (Method validation and quality control procedures for pesticide residues analysis in food and feed), two product ions were selected for the LC-MS/MS method, whereas mass accuracy < 5 ppm was the target for LC-HRMS detection.
Feasibility study of inclusion of mixtures of pesticides in white wine matrix
B Ciasca;A Visconti
2015
Abstract
The aim of this study was the evaluation of compatibility of mixtures of pesticides with white wine matrix in order to establish that all the criteria for a candidate reference material were met (homogeneity, stability, definition of certified property values and related uncertainties). The matrix selected for this assay was a pesticide free white wine (i.e. containing selected pesticides at levels lower than the relevant limit of detection, L.O.D.). The spiking mixtures to be included in the matrix were composed by a selection of pesticides usually found in viticulture, belonging to different chemical classes and characterized by specific mode of action. According to CIPAC Method MT 46, the matrices spiked with pesticide mixtures were stressed at 54°C for 14 days in order to investigate on the achievable long-term stability. Pesticide mixtures were analyzed by liquid chromatography tandem mass spectrometry (LC-MS/MS) evaluating the intrinsic amenability to this analytical technique for every single compound and taking into account data of annex B of European EN 15662:2009 "Foods of plant origin - Determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by dispersive SPE - QuEChERS-method". White wine is a high water content matrix (80-100%) and contains a variable amount of carbohydrates and organic acids. Therefore extraction and clean-up were performed according to QuEChERS procedure, according to annex C of EN 15662:2009. The quantitative determination of pesticides in the wine matrix mixture was accomplished by LC-MS/MS and LC-HRMS based in Orbitrap technology. Tuning of instrumental parameters for the multiresidue method, either LC-MS/MS and LC-HRMS settings, was performed by direct infusion of every single pesticide. Data were acquired in Selected Reaction Monitoring mode for LC-MS/MS and HR Full Scan mode for LC-HRMS. In order to fulfill the requirements specified in the document SANCO 10684/2013 (Method validation and quality control procedures for pesticide residues analysis in food and feed), two product ions were selected for the LC-MS/MS method, whereas mass accuracy < 5 ppm was the target for LC-HRMS detection.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
