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eLibrary > BS EN 15662:2018 Foods of plant origin. Multimethod for the determination of pesticide residues using GC- and LC-based analysis following acetonitrile extraction/partitioning and clean-up by dispersive SPE. Modular QuEChERS-method >

BS EN 15662:2018 Foods of plant origin. Multimethod for the determination of pesticide residues using GC- and LC-based analysis following acetonitrile extraction/partitioning and clean-up by dispersive SPE. Modular QuEChERS-method, 2018

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BS EN 15662:2018 Foods of plant origin. Multimethod for the determination of pesticide residues using GC- and LC-based analysis following acetonitrile extraction/partitioning and clean-up by dispersive SPE. Modular QuEChERS-method, 2018

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1 Scope
2 Normative references
3 Principle
4 Preparation and storage of the samples [Go to Page]
4.1 General
4.2 Laboratory sample
4.3 Partly-prepared test sample
4.4 Test sample
4.5 Test portion
5 Procedure
6 Evaluation of results [Go to Page]
6.1 Identification and quantification
6.2 Calibration
6.3 Calculation of residue concentration
6.4 Validity of the method
7 Confirmatory tests
8 Precision
9 Test report
Annex A (informative)Description of modules [Go to Page]
A.1 Reagents used in all extraction (E) and clean-up (C) and stabilization (S) modules
A.2 Apparatus used in all extraction (E) and clean-up (C) and stabilization (S) modules
A.3 Description of extraction (E) modules [Go to Page]
A.3.1 Module E1: Extraction of a 10 g test portion without additional water using acetonitrile [Go to Page]
A.3.1.1 Principle
A.3.1.2 Procedure
A.3.1.3 Calculation
A.3.1.4 Flowchart of module E1
A.3.2 Module E2: Extraction of a 10 g test portion without additional water after addition of a) 0,6 ml or b) 0,2 ml of 5 mol/l sodium hydroxide solution using acetonitrile [Go to Page]
A.3.2.1 Principle
A.3.2.2 Procedure
A.3.2.3 Calculation
A.3.2.4 Flowchart of module E2
A.3.3 Module E3: Extraction of a 10 g test portion after addition of a) 2,5 ml or b) 4,5 ml of water using acetonitrile [Go to Page]
A.3.3.1 Principle
A.3.3.2 Procedure
A.3.3.3 Calculation
A.3.3.4 Flowchart of module E3
A.3.4 Module E4: Homogenization of the sample with addition of water, extraction of a 13,5 g homogenate using acetonitrile [Go to Page]
A.3.4.1 Principle
A.3.4.2 Procedure
A.3.4.3 Calculation
A.3.4.4 Flowchart of module E4
A.3.5 Module E5: Extraction of a 5 g test portion after addition of 10 ml of water using acetonitrile [Go to Page]
A.3.5.1 Principle
A.3.5.2 Procedure
A.3.5.3 Calculation
A.3.5.4 Flowchart of module E5
A.3.6 Module E6: Extraction of a 5 g test portion after addition of 6 ml of water using acetonitrile [Go to Page]
A.3.6.1 Principle
A.3.6.2 Procedure
A.3.6.3 Calculation
A.3.6.4 Flowchart of module E6
A.3.7 Module E7: Extraction of a 2 g test portion after addition of 10 ml of water using acetonitrile [Go to Page]
A.3.7.1 Principle
A.3.7.2 Procedure
A.3.7.3 Calculation
A.3.7.4 Flowchart of module E7
A.3.8 Module E8: Extraction of a 10 g test portion without additional water with simultaneous alkaline hydrolysis of alkaline labile esters and conjugates using acetonitrile [Go to Page]
A.3.8.1 Principle
A.3.8.2 Procedure
A.3.8.3 Calculation
A.3.8.4 Flowchart of module E8
A.3.9 Module E9: Extraction of 2 g or 5 g test portions after addition of water with simultaneous alkaline hydrolysis of alkaline labile esters and conjugates using acetonitrile [Go to Page]
A.3.9.1 Principle
A.3.9.2 Procedure
A.3.9.3 Calculation
A.3.9.4 Flowchart of module E9
A.4 Description of clean-up (C) modules [Go to Page]
A.4.1 Module C0: No clean-up [Go to Page]
A.4.1.1 Principle
A.4.1.2 Procedure
A.4.1.3 Calculation
A.4.1.4 Flowchart of module C0
A.4.2 Module C1: Clean-up by freezing-out of co-extracted fat, wax, sugars [Go to Page]
A.4.2.1 Principle
A.4.2.2 Procedure
A.4.2.3 Calculation
A.4.2.4 Flowchart of module C1
A.4.3 Module C2: Clean-up by dispersive SPE with amine sorbent (PSA) [Go to Page]
A.4.3.1 Principle
A.4.3.2 Procedure
A.4.3.3 Calculation
A.4.3.4 Flowchart of module C2
A.4.4 Module C3: Clean-up by dispersive SPE with a larger amount of amine sorbent (PSA) a) 50 mg PSA/ml extract or b) 75 mg PSA/ml extract) [Go to Page]
A.4.4.1 Principle
A.4.4.2 Procedure
A.4.4.3 Calculation
A.4.4.4 Flowchart of module C3
A.4.5 Module C4: Clean-up by dispersive SPE with a mixture of amine sorbent (PSA) and silica based reverse phase sorbent (C18) [Go to Page]
A.4.5.1 Principle
A.4.5.2 Procedure
A.4.5.3 Calculation
A.4.5.4 Flowchart of module C4
A.4.6 Module C5: Clean-up by dispersive SPE with a mixture of amine sorbent (PSA) and graphitized carbon black [Go to Page]
A.4.6.1 Principle
A.4.6.2 Procedure
A.4.6.3 Calculation
A.4.6.4 Flowchart of module C5
A.5 Description of extract stabilization (S) modules [Go to Page]
A.5.1 Module S0: No extract stabilization [Go to Page]
A.5.1.1 Principle
A.5.1.2 Procedure
A.5.1.3 Flowchart of module S0
A.5.2 Module S1: Extract stabilization with formic acid [Go to Page]
A.5.2.1 Principle
A.5.2.2 Procedure
A.5.2.3 Flowchart of module S1
A.6 Description of detection (D) modules [Go to Page]
A.6.1 Module D1: Determination using liquid chromatography with tandem-mass spectrometric detection (LC-MS/MS) [Go to Page]
A.6.1.1 Principle
A.6.1.2 Procedure
A.6.1.3 Apparatus
A.6.1.4 Examples of suitable conditions
A.6.1.5 Procedural remarks
A.6.2 Module D2: Determination using liquid chromatography with accurate mass spectrometric detection (LC-accurate mass) [Go to Page]
A.6.2.1 Principle
A.6.2.2 Procedure
A.6.2.3 Apparatus
A.6.2.4 Examples of suitable conditions
A.6.2.5 Procedural remarks
A.6.3 Module D3: Determination using gas chromatography with tandem-mass spectrometric detection (GC-MS/MS) [Go to Page]
A.6.3.1 Principle
A.6.3.2 Procedure
A.6.3.3 Apparatus
A.6.3.4 Examples of suitable conditions
A.6.3.5 Procedural remarks
A.6.4 Module D4: Determination using gas chromatography with mass spectrometric detection (GC-MS) [Go to Page]
A.6.4.1 Principle
A.6.4.2 Procedure
A.6.4.3 Apparatus
A.6.4.4 Examples of suitable conditions
A.6.4.5 Procedural remarks
A.6.5 Module D5: Determination using gas chromatography with flame photometric detection (GC-FPD) [Go to Page]
A.6.5.1 Principle
A.6.5.2 Procedure
A.6.5.3 Apparatus
A.6.5.4 Examples of suitable conditions
A.6.6 Module D6: Determination using gas chromatography with electron capture detection (GC-ECD) [Go to Page]
A.6.6.1 Principle
A.6.6.2 Procedure
A.6.6.3 Apparatus
A.6.6.4 Examples of suitable conditions
A.7 Description of quantification (Q) options [Go to Page]
A.7.1 Option Q1: Quantification using external standards in solvent [Go to Page]
A.7.1.1 Principle
A.7.1.2 Procedure
A.7.1.3 Calculation
A.7.2 Option Q2: Quantification using external standards in matrix [Go to Page]
A.7.2.1 Principle
A.7.2.2 Procedure
A.7.2.3 Calculation
A.7.3 Option Q3: Quantification using a procedural internal standard and standards in solvent [Go to Page]
A.7.3.1 Principle
A.7.3.2 Procedure
A.7.3.3 Calculation
A.7.4 Option Q4: Quantification using standard addition to the final extract [Go to Page]
A.7.4.1 Principle
A.7.4.2 Procedure
A.7.4.3 Calculation
A.7.5 Option Q5: Quantification using a procedural internal standard and standards in matrix or isotope-labelled internal standards [Go to Page]
A.7.5.1 Principle
A.7.5.2 Procedure
A.7.5.3 Calculation
A.7.6 Option Q6: Quantification using standard addition to the sample [Go to Page]
A.7.6.1 Principle
A.7.6.2 Procedure
A.7.6.3 Calculation
A.7.7 Option Q7: Quantification by calibration of the entire procedure [Go to Page]
A.7.7.1 Principle
A.7.7.2 Procedure
A.7.7.3 Calculation
Annex B (informative)Complementary information [Go to Page]
B.1 General
B.2 Preparation of the buffer-salt mixture (A.1.8)
B.3 Reagents for clean-up
B.4 Prolongation of extraction time
B.5 Working without internal standards
B.6 Scaling
B.7 Adjustment of pH value
B.8 Recovery studies
B.9 Clean-up with GCB
B.10 Concentration of the final extracts and solvent exchange
Annex C (informative)Abbreviations [Go to Page]

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BS EN 15662:2018 Foods of plant origin. Multimethod for the determination of pesticide residues using GC- and LC-based analysis following acetonitrile extraction/partitioning and clean-up by dispersive SPE. Modular QuEChERS-method, 2018

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BS EN 15662:2018 Foods of plant origin. Multimethod for the determination of pesticide residues using GC- and LC-based analysis following acetonitrile extraction/partitioning and clean-up by dispersive SPE. Modular QuEChERS-method, 2018

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