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BSI 23/30481845 DC:2023 Edition

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EN 18032 Foodstuff. Quick Method for the Analysis of Multiple Highly Polar Pesticides and their Metabolites in Foodstuff Involving Extraction with Acidified Methanol and Measurement by LC- or IC-MS/MS (QuPPe-Method)

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BSI 2023 87
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This document specifies a procedure for the analysis of residues of highly polar pesticides and metabolites, which are not amenable to common multiresidue methods, in various food commodities of plant and animal origin, including fruits, vegetables, cereals, pulses, oily seeds, nuts, milk, liver and honey. The method was developed at the EURL-SRM hosted at CVUA Stuttgart and has been collaboratively studied on a large number of commodity/pesticide combinations. Guidelines for calibration are outlined in CEN/TS 17061:2019.

PDF Catalog

PDF Pages PDF Title
1 30481845-NC.pdf
3 41_e_stf (2).pdf
6 1 Scope
2 Normative references
3 Terms and Definitions
4 Principle
5 Preparation and storage of the samples
5.1 General considerations
7 5.2 Laboratory sample
5.3 Treatment of laboratory samples prior to milling
5.4 Sample homogenization
5.4.1 General considerations
8 5.4.2 Preparation of homogenates of dried fruit and similar commodities
5.5 Analytical test portion
9 6 Procedure
22 7 Evaluation of results
7.1 Identification
7.2 Calibration and quantification
23 7.3 Calculation of residue levels
7.3.1 Calculation of residue concentrations using external calibration without IL-ISs
24 7.3.2 Calculation of residue concentrations using external calibration and IL-IS
25 7.3.3 Calculation of residue concentration using the standard additions approach
7.3.4 Calculation of residue levels of complex residue definitions
8 Validity of the method
30 9 Test report
10 Additional information on analysis
10.1 Extraction Time
10.2 Scaling
31 Annex A (informative)Description of modules
A.1.1 Water, deionized, for water additions to the samples
A.1.2 Water, ultrapure, e.g. prepared by a laboratory water purification system
A.1.3 Methanol, at least HPLC quality, for the preparation of mobile phases preferably use MS-quality methanol
A.1.4 Acetonitrile, at least HPLC quality, for the preparation of mobile phases preferably use MS-quality acetonitrile
A.1.5 Formic acid, concentrated, > 98 %, for the preparation of mobile phases preferably use MS-quality formic acid
A.1.6 Acetic Acid, concentrated, > 98 %, for the preparation of mobile phases preferably use MS-quality acetic acid
A.1.7 Acidified methanol, for the extraction of the majority of samples
A.1.8 C18 bulk sorbent, 30 µm to 300 µm particle size (also known as ODS-sorbent)
A.1.9 Ammonium formate, p.a
A.1.10 Ethylenediaminetetraacetic acid tetrasodium, Na4-EDTA
A.1.11 Na4-EDTA solution, 10 %, aqueous (EDTA-solution)
32 A.1.12 Cryogenic milling aid, e.g. dry ice or liquid nitrogen.
A.1.13 Pesticide Standards, of known purity
A.1.14 Internal Standards (IL-ISs).
A.1.15 LC-MS/MS mobile phases.
A.1.16 Pesticide stock solutions.
A.1.17 Pesticide working solutions/ mixtures.
A.1.18 Internal Standards (IL-ISs) and IL-IS-stock solutions.
33 A.1.19 IL-IS-working solution I (IL-IS-WSln-1), for spiking samples prior to extraction
A.1.20 IL-IS-working solution II (IL-IS-WSln-2), for preparation of calibration standards
34 A.1.21 Blank extracts, used for preparation of standard solutions
A.1.22 Standard solutions for calibration, solvent-based, matrix-based and matrix-matched
36 A.1.23 Solutions for approach of standard-additions to extract aliquots.
37 A.2.1 Powerful sample processing equipment, for milling samples
A.2.2 High-performance dispersing device, for homogenization or supported extraction
A.2.3 Stainless steel grinding balls, diameter 7 mm to 10 mm
A.2.4 Centrifuge tubes with screw caps, capacity of 50 ml
A.2.5 Centrifuge tubes with screw caps, capacity of 10 ml, for the d-SPE step (A.4.4)
A.2.6 Automatic pipettes, suitable for handling volumes of 10 µl to 100 μl, 200 μl to 1 000 μl and 1 µl to 10 ml
A.2.7 Solvent-dispenser, capacity of 10 ml, for acidified methanol (A.1.7)
A.2.8 Mechanical shaking device, e.g. suitable for 50 ml centrifuge tubes
A.2.9 Centrifuge, suitable for the centrifuge tubes employed in the procedure and capable of achieving > 3 000 g
38 A.2.10 Disposable syringes, suitable to the filters used
A.2.11 Disposable syringe filters, particle filters
A.2.12 Ultrafiltration filters, 5 kDa or 10 kDa molecular weight cut-off filters suitable for centrifuges
A.2.13 Autosampler vials, suitable for LC and IC auto-samplers
A.2.14 Volumetric flask with stoppers, for the preparation of stock and working solutions, e.g. 20 ml, 25 ml, 50 ml, 100 ml glass flasks
A.2.15 Plastic vessel, for the storage of stock or working solutions and storage of extracts, e.g. 15 ml vessels of polypropylene with screw closure
A.2.16 LC-MS/MS instrumentation, equipped with ESI source and appropriate columns
A.2.17 IC-MS/MS instrumentation, equipped with ESI source and appropriate columns
A.3.1 General
48 A.5.1 Short description
A.5.2 Procedure
49 A.5.3 Calculation
A.6.1 General
A.6.2 Module M1: LC-MS/MS (HILIC-column, ESI neg. mode)
A.6.2.1 Short description
A.6.2.2 Procedure
A.6.2.3 Instrumental Parameters
52 A.6.3 Module M2: LC-MS/MS (HILIC-column, ESI pos. mode)
A.6.3.1 Short description
53 A.6.3.2 Procedure
A.6.3.3 Instrumental Parameters
54 A.6.4 Module M3: LC-MS/MS (porous graphitic carbon column, ESI neg. mode)
A.6.4.1 Short description
A.6.4.2 Procedure
A.6.4.3 Instrumental Parameters
55 A.6.5 Module M4: IC-MS/MS (anion exchange column, ESI neg. mode)
A.6.5.1 Short description
A.6.5.2 Procedure
56 A.6.5.3 Instrumental Parameters
A.6.6 Module M5: IC-MS/MS (cation exchange column, ESI pos. mode)
A.6.6.1 Short description
57 A.6.6.2 Procedure
A.6.6.3 Instrumental Parameters
58 A.6.7 MS-Conditions: Details and general remarks
A.6.7.1 MS-instrument parameters for measurements in ESI neg. mode
60 A.6.7.2 MS-instrument parameters for measurements in ESI pos. mode
62 A.6.7.3 Compound mass transitions and remarks (ESI neg. mode)
67 A.6.7.4 Compound mass transitions and hints (ESI pos.)
77 Annex B (normative)Additional information
85 Annex C (informative)Overview of “Online Supplement”
BSI 23/30481845 DC
$13.70