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BS EN 18032:2025 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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BS EN 18032:2025 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), 2025
- undefined
- European foreword
- 1 Scope
- 2 Normative references
- 3 Terms and definitions
- 4 Principle
- 5 Preparation and storage of the samples [Go to Page]
- Table 1 — Dried fruits/water proportion during homogenization [Go to Page]
- 6 Procedure
- Table 2 — Extraction modules
- Table 3 — Clean-up modules
- Table 4 — Dilution modules - exemplary
- Table 5 — Measurement modules
- Table 6 — Quantification modules
- 7 Evaluation of results [Go to Page]
- 8 Validity of the method
- Table 7 — Overview of available validation data generated within the frame of inter-laboratory validation studies (successful validation by ≥ 3 laboratories with n = 5 for 2 levels)
- Table 8 — Overview of currently applying MRLs for commodities of plant origin and comparison to the lowest successfully validated levels (LSVLs) within the inter-laboratory study, status as of DATE [11]
- Table 9 — Overview of currently applying MRLs for commodities of animal origin and comparison to the lowest successfully validated levels (LSVLs) within the inter-laboratory study, status as of [11]
- 9 Test report
- 10 Additional information on analysis [Go to Page]
- Annex A (informative) Description of modules
- A.1 Reagents
- Table A.1 — Exemplary concentrations of IL-IS Working Solutions (IL-IS-WSln)
- Table A.2 — Exemplary pipetting scheme for the preparation of calibration standards
- Table A.3 — Exemplary pipetting scheme for standard additions to extract aliquots
- A.2 Apparatuses and utensils
- A.3 Extraction (E) modules
- A.3.1 General
- A.3.2 Module E1: Extraction of 10 g sample with ≥ 80 % moisture
- A.3.2.1 Short description
- A.3.2.2 Procedure
- A.3.2.2.1 Weighing of analytical test portion and water adjustment
- A.3.2.2.2 Addition of IL-IS (recommended)
- A.3.2.2.3 Extraction and centrifugation
- A.3.3 Module E2: Extraction of 10 g sample with 40 % to 80 % moisture, after addition of water
- A.3.3.1 Short description
- A.3.3.2 Procedure
- A.3.3.2.1 Weighing of the analytical test portion and water adjustment
- A.3.3.2.2 Addition of IL-IS (recommended)
- A.3.3.2.3 Extraction and Centrifugation
- A.3.4 Module E3: Extraction of a re-hydratized homogenate of samples with an original moisture content between 15 % and 40 %,
- A.3.4.1 Short description
- A.3.4.2 Procedure
- A.3.4.2.1 Weighing of analytical portion
- A.3.4.2.2 Addition of IL-IS (recommended)
- A.3.4.2.3 Extraction and Centrifugation
- A.3.5 Module E4: Honey
- A.3.5.1 Short description
- A.3.5.2 Procedure
- A.3.5.2.1 Weighing of analytical test portion
- A.3.5.2.2 Addition of IL-IS (recommended)
- A.3.5.2.3 Extraction and Centrifugation
- A.3.6 Module E5a: Extraction of 2 g or 5 g sample with a moisture content < 15 %, after addition of 10 ml water
- A.3.6.1 Short description
- A.3.6.2 Procedure
- A.3.6.2.1 Weighing of analytical test portion and water adjustment
- A.3.6.2.2 Addition of IL-IS (recommended)
- A.3.6.2.3 Extraction and Centrifugation
- A.3.7 Module E5b: Extraction of 2 g or 5 g samples with a moisture content < 15 %, after addition of water, 10 % EDTA and formic acid
- A.3.7.1 Short description
- A.3.7.2 Procedure
- A.3.7.2.1 Weighing of analytical test portion and water adjustment
- A.3.7.2.2 Addition of IL-IS (recommended)
- A.3.7.2.3 Extraction, Centrifugation and Filtration
- A.3.8 Module E6a: Extraction of 10 g sample of animal origin with a moisture content > 30 %, after addition of water
- A.3.8.1 Short description
- A.3.8.2 Procedure
- A.3.8.2.1 Weighing of analytical test portion and adjustment of water
- A.3.8.2.2 Addition of IL-IS (recommended)
- A.3.8.2.3 Extraction and Centrifugation
- A.3.9 Module E6b: Extraction of 10 g sample of animal origin with a moisture content > 30 %, after addition of water, 10 % EDTA and formic acid
- A.3.9.1 Short description
- A.3.9.2 Procedure
- A.3.9.2.1 Weighing of analytical test portion and adjustment of water
- A.3.9.2.2 Addition of IL-IS (recommended)
- A.3.9.2.3 Extraction and Centrifugation
- A.3.10 Module E7: Extraction of 5 g fat samples, with the help of mechanical aids
- A.3.10.1 Short description
- A.3.10.2 Procedure
- A.3.10.2.1 Weighing of analytical test portion
- A.3.10.2.2 Addition of IL-IS (recommended)
- A.3.10.2.3 Extraction, Centrifugation and Filtration
- A.4 Clean-up (C) modules
- A.4.1 General
- A.4.2 Module C0: No clean-up
- A.4.3 Module C1: Freeze-out for the precipitation of poorly soluble co-extractives
- A.4.3.1 Short description
- A.4.3.2 Procedure
- A.4.4 Module C2: Dispersive SPE with C18-sorbent
- A.4.4.1 Short description
- A.4.4.2 Procedure
- A.4.5 Module C3a: Precipitation with acetonitrile
- A.4.5.1 Short description
- A.4.5.2 Procedure
- A.4.6 Module C3b: Precipitation with acetonitrile combined with C18 sorbent
- A.4.6.1 Short description
- A.4.6.2 Procedure
- A.4.7 Module C4: Ultrafiltration using cut-off filters of 5 kDa or 10 kDa (optional)
- A.4.7.1 Short description
- A.4.7.2 Procedure
- A.5 Dilution (DL) Modules
- A.5.1 Short description
- A.5.2 Procedure
- A.5.3 Calculation
- A.6 Measurement (M) Modules
- 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
- A.6.2.3.1 General
- A.6.2.3.2 Exemplary LC Parameters, M1a (HILIC, ESI-neg.)
- Table A.4
- A.6.2.3.3 Exemplary LC Parameters, M1b (HILIC, ESI-neg.)
- Table A.5
- A.6.2.3.4 Exemplary LC Parameters, M1c (HILIC, ESI-neg.)
- Table A.6
- A.6.2.3.5 Exemplary LC Parameters, M1d (HILIC, ESI-neg.)
- Table A.7
- A.6.2.3.6 Exemplary LC Parameters, M1e (HILIC, ESI-neg.)
- Table A.8
- A.6.2.3.7 Exemplary LC Parameters, M1f (HILIC, ESI-neg.)
- Table A.9
- A.6.3 Module M2: LC-MS/MS (HILIC-column, ESI pos. mode)
- A.6.3.1 Short description
- A.6.3.2 Procedure
- A.6.3.3 Instrumental Parameters
- A.6.3.3.1 General
- A.6.3.3.2 Exemplary LC Parameters, M2a (HILIC, ESI-pos.)
- Table A.10
- A.6.3.3.3 Exemplary LC Parameters, M2b (HILIC, ESI-pos.)
- Table A.11
- A.6.3.3.4 Exemplary LC Parameters, M2c (HILIC, ESI-pos.)
- Table A.12
- A.6.3.3.5 Exemplary LC Parameters, M2d (HILIC, ESI-pos.)
- Table A.13
- 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
- A.6.4.3.1 General
- A.6.4.3.2 Exemplary LC Parameters, M3a (PGC, ESI-neg.)
- Table A.14
- A.6.4.3.3 Exemplary LC Parameters, M3b (PGC, ESI-neg.)
- Table A.15
- 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
- A.6.5.3 Instrumental Parameters
- A.6.5.3.1 General
- A.6.5.3.2 Exemplary IC Parameters, M4a (Anion Exchange, ESI-neg.)
- Table A.16
- A.6.5.3.3 Exemplary IC Parameters, M4b (Anion Exchange, ESI-neg.)
- Table A.17
- A.6.6 Module M5: IC-MS/MS (cation exchange column, ESI pos. mode)
- A.6.6.1 Short description
- A.6.6.2 Procedure
- A.6.6.3 Instrumental Parameters
- A.6.6.3.1 General
- A.6.6.3.2 Exemplary IC Parameters, M5a (Cation Exchange, ESI-pos.)
- Table A.18
- A.6.6.3.3 Exemplary IC Parameters, M5b (Cation Exchange, ESI-pos.)
- Table A.19
- A.6.7 MS-Conditions: Details and general remarks
- A.6.7.1 MS-instrument parameters for measurements in ESI neg. mode
- A.6.7.1.1 General
- A.6.7.1.2 Exemplary MS parameters ESI-neg. A
- Table A.20
- A.6.7.1.3 Exemplary MS parameters ESI-neg. B
- Table A.21
- A.6.7.1.4 Exemplary MS parameters ESI-neg. C
- Table A.22
- A.6.7.1.5 Exemplary MS parameters ESI-neg. D
- Table A.23
- A.6.7.1.6 Exemplary MS parameters ESI-neg. E
- Table A.24
- A.6.7.1.7 Exemplary MS parameters ESI-neg. F
- Table A.25
- A.6.7.2 MS-instrument parameters for measurements in ESI pos. mode
- A.6.7.2.1 General
- A.6.7.2.2 Exemplary MS parameters ESI-pos. A
- Table A.26
- A.6.7.2.3 Exemplary MS parameters ESI-pos. B
- Table A.27
- A.6.7.2.4 Exemplary MS parameters ESI-pos. C
- Table A.28
- A.6.7.3 Compound mass transitions and remarks (ESI neg. mode)
- Table A.29
- A.6.7.4 Compound mass transitions and hints (ESI pos.)
- Table A.30
- A.7 Quantification (Q) Modules
- A.7.1 Module Q1a: Quantification using calibration based on external standards in solvent (solvent-based without the use of IL-IS)
- A.7.1.1 General
- A.7.1.2 Procedure
- A.7.1.3 Calibration and calculation
- A.7.2 Module Q1b: Quantification using calibration based on external standards in solvent and IL-IS (solvent-based calibration using IL-IS)
- A.7.2.1 General
- A.7.2.2 Procedure
- A.7.2.3 Calibration and calculation
- A.7.3 Module Q2a: Quantification using calibration based on external standards in extracts of generic residue-free samples (matrix based calibration without the use of IL-IS)
- A.7.3.1 General
- A.7.3.2 Procedure
- A.7.3.3 Calibration and calculation
- A.7.4 Module Q2b: Quantification using calibration based on external standards in extracts of generic residue-free samples and IL-IS (matrix-based calibration using IL-IS)
- A.7.4.1 General
- A.7.4.2 Procedure
- A.7.4.3 Calibration and calculation
- A.7.5 Module Q3a: Quantification using calibration based on external standards in extracts of residue-free samples of the same matrix type (matrix matched calibration without the use of IL-IS)
- A.7.5.1 General
- A.7.5.2 Procedure
- A.7.5.3 Calibration and calculation
- A.7.6 Module Q3b: Quantification using calibration based on external standards in extracts of residue-free samples of the same matrix type, with IL-IS (matrix-matched calibration using IL-IS)
- A.7.6.1 General
- A.7.6.2 Procedure
- A.7.6.3 Calibration and calculation
- A.7.7 Module Q4a: Quantification using external standards spiked on portions of residue-free control samples and passing through the entire procedure not using IL-IS, (procedural calibration without IL-IS)
- A.7.7.1 General
- A.7.7.2 Procedure
- A.7.7.3 Calibration and calculation
- A.7.8 Module Q4b: Quantification using external standards spiked on portions of residue-free control samples and passing through the entire procedure using IL-IS, (procedural calibration using IL-IS)
- A.7.8.1 General
- A.7.8.2 Procedure
- A.7.8.3 Calibration and calculation
- A.7.9 Module Q5: Quantification using standard addition to the final extract (optionally using IL-IS if available) (standard additions on extract aliquots)
- A.7.9.1 General
- A.7.9.2 Procedure
- A.7.9.3 Calibration and calculation
- A.7.10 Module Q6: Quantification using standard addition to separate test portions of the sample (optionally using IL-IS if available) (standard additions on sample portions)
- A.7.10.1 General
- A.7.10.2 Procedure
- A.7.10.3 Calculation
- Annex B (normative) Additional information
- Table B.1 — Preferred combinations of E and C modules for exemplary commodities
- Annex C (informative) Supplementary information on the method
- Annex D (informative) Abbreviations and symbols
- Table D.1 — List of abbreviations and symbols
- Bibliography [Go to Page]