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23/30481845 DC 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), 2023
- 30481845-NC.pdf
- 41_e_stf (2).pdf [Go to Page]
- 1 Scope
- 2 Normative references
- 3 Terms and Definitions
- 4 Principle
- 5 Preparation and storage of the samples [Go to Page]
- 5.1 General considerations
- 5.2 Laboratory sample
- 5.3 Treatment of laboratory samples prior to milling
- 5.4 Sample homogenization [Go to Page]
- 5.4.1 General considerations
- 5.4.2 Preparation of homogenates of dried fruit and similar commodities
- 5.5 Analytical test portion
- 6 Procedure
- 7 Evaluation of results [Go to Page]
- 7.1 Identification
- 7.2 Calibration and quantification
- 7.3 Calculation of residue levels [Go to Page]
- 7.3.1 Calculation of residue concentrations using external calibration without IL-ISs
- 7.3.2 Calculation of residue concentrations using external calibration and IL-IS
- 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
- 9 Test report
- 10 Additional information on analysis [Go to Page]
- 10.1 Extraction Time
- 10.2 Scaling
- Annex A (informative)Description of modules [Go to Page]
- 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)
- 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.
- 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
- 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
- A.1.23 Solutions for approach of standard-additions to extract aliquots.
- 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
- 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
- A.5.1 Short description
- A.5.2 Procedure
- A.5.3 Calculation
- A.6.1 General
- A.6.2 Module M1: LC-MS/MS (HILIC-column, ESI neg. mode) [Go to Page]
- A.6.2.1 Short description
- A.6.2.2 Procedure
- A.6.2.3 Instrumental Parameters
- A.6.3 Module M2: LC-MS/MS (HILIC-column, ESI pos. mode) [Go to Page]
- A.6.3.1 Short description
- A.6.3.2 Procedure
- A.6.3.3 Instrumental Parameters
- A.6.4 Module M3: LC-MS/MS (porous graphitic carbon column, ESI neg. mode) [Go to Page]
- A.6.4.1 Short description
- A.6.4.2 Procedure
- A.6.4.3 Instrumental Parameters
- A.6.5 Module M4: IC-MS/MS (anion exchange column, ESI neg. mode) [Go to Page]
- A.6.5.1 Short description
- A.6.5.2 Procedure
- A.6.5.3 Instrumental Parameters
- A.6.6 Module M5: IC-MS/MS (cation exchange column, ESI pos. mode) [Go to Page]
- A.6.6.1 Short description
- A.6.6.2 Procedure
- A.6.6.3 Instrumental Parameters
- A.6.7 MS-Conditions: Details and general remarks [Go to Page]
- A.6.7.1 MS-instrument parameters for measurements in ESI neg. mode
- A.6.7.2 MS-instrument parameters for measurements in ESI pos. mode
- A.6.7.3 Compound mass transitions and remarks (ESI neg. mode)
- A.6.7.4 Compound mass transitions and hints (ESI pos.)
- Annex B (normative)Additional information
- Annex C (informative)Overview of “Online Supplement” [Go to Page]
