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BS EN 15662:2018

BS EN 15662:2018

$215.11

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

Published By Publication Date Number of Pages
BSI 2018 84
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This European Standard stipulates a method for the analysis of pesticide residues in foods of plant origin, such as fruits (including dried fruits), vegetables (including dried vegetables), cereals and many processed products thereof by using GC, GC-MS(/MS), and/or LC-MS(/MS). The method has been collaboratively studied on a large number of commodity/pesticide combinations. Precision data are summarized in CEN/TR 17063. Guidelines for calibration are outlined in CEN/TS 17061.

PDF Catalog

PDF Pages PDF Title
2 undefined
6 1 Scope
2 Normative references
3 Principle
4 Preparation and storage of the samples
4.1 General
4.2 Laboratory sample
7 4.3 Partly-prepared test sample
4.4 Test sample
4.5 Test portion
5 Procedure
17 6 Evaluation of results
6.1 Identification and quantification
6.2 Calibration
6.3 Calculation of residue concentration
18 6.4 Validity of the method
24 7 Confirmatory tests
8 Precision
9 Test report
25 Annex A (informative)Description of modules
A.1 Reagents used in all extraction (E) and clean-up (C) and stabilization (S) modules
28 A.2 Apparatus used in all extraction (E) and clean-up (C) and stabilization (S) modules
A.3 Description of extraction (E) modules
A.3.1 Module E1: Extraction of a 10 g test portion without additional water using acetonitrile
A.3.1.1 Principle
29 A.3.1.2 Procedure
A.3.1.3 Calculation
30 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
A.3.2.1 Principle
31 A.3.2.2 Procedure
A.3.2.3 Calculation
32 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
A.3.3.1 Principle
33 A.3.3.2 Procedure
A.3.3.3 Calculation
34 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
A.3.4.1 Principle
35 A.3.4.2 Procedure
A.3.4.3 Calculation
36 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
A.3.5.1 Principle
37 A.3.5.2 Procedure
A.3.5.3 Calculation
38 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
A.3.6.1 Principle
39 A.3.6.2 Procedure
A.3.6.3 Calculation
40 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
A.3.7.1 Principle
41 A.3.7.2 Procedure
A.3.7.3 Calculation
42 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
A.3.8.1 Principle
43 A.3.8.2 Procedure
A.3.8.3 Calculation
44 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
A.3.9.1 Principle
45 A.3.9.2 Procedure
46 A.3.9.3 Calculation
A.3.9.4 Flowchart of module E9
47 A.4 Description of clean-up (C) modules
A.4.1 Module C0: No clean-up
A.4.1.1 Principle
A.4.1.2 Procedure
A.4.1.3 Calculation
48 A.4.1.4 Flowchart of module C0
A.4.2 Module C1: Clean-up by freezing-out of co-extracted fat, wax, sugars
A.4.2.1 Principle
A.4.2.2 Procedure
A.4.2.3 Calculation
49 A.4.2.4 Flowchart of module C1
A.4.3 Module C2: Clean-up by dispersive SPE with amine sorbent (PSA)
A.4.3.1 Principle
A.4.3.2 Procedure
50 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)
A.4.4.1 Principle
51 A.4.4.2 Procedure
A.4.4.3 Calculation
52 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)
A.4.5.1 Principle
A.4.5.2 Procedure
A.4.5.3 Calculation
53 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
A.4.6.1 Principle
54 A.4.6.2 Procedure
A.4.6.3 Calculation
55 A.4.6.4 Flowchart of module C5
A.5 Description of extract stabilization (S) modules
A.5.1 Module S0: No extract stabilization
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
A.5.2.1 Principle
A.5.2.2 Procedure
56 A.5.2.3 Flowchart of module S1
A.6 Description of detection (D) modules
A.6.1 Module D1: Determination using liquid chromatography with tandem-mass spectrometric detection (LC-MS/MS)
A.6.1.1 Principle
A.6.1.2 Procedure
A.6.1.3 Apparatus
A.6.1.4 Examples of suitable conditions
59 A.6.1.5 Procedural remarks
60 A.6.2 Module D2: Determination using liquid chromatography with accurate mass spectrometric detection (LC-accurate mass)
A.6.2.1 Principle
A.6.2.2 Procedure
A.6.2.3 Apparatus
A.6.2.4 Examples of suitable conditions
64 A.6.2.5 Procedural remarks
65 A.6.3 Module D3: Determination using gas chromatography with tandem-mass spectrometric detection (GC-MS/MS)
A.6.3.1 Principle
A.6.3.2 Procedure
A.6.3.3 Apparatus
A.6.3.4 Examples of suitable conditions
67 A.6.3.5 Procedural remarks
68 A.6.4 Module D4: Determination using gas chromatography with mass spectrometric detection (GC-MS)
A.6.4.1 Principle
A.6.4.2 Procedure
A.6.4.3 Apparatus
69 A.6.4.4 Examples of suitable conditions
70 A.6.4.5 Procedural remarks
A.6.5 Module D5: Determination using gas chromatography with flame photometric detection (GC-FPD)
A.6.5.1 Principle
A.6.5.2 Procedure
71 A.6.5.3 Apparatus
A.6.5.4 Examples of suitable conditions
72 A.6.6 Module D6: Determination using gas chromatography with electron capture detection (GC-ECD)
A.6.6.1 Principle
A.6.6.2 Procedure
A.6.6.3 Apparatus
A.6.6.4 Examples of suitable conditions
74 A.7 Description of quantification (Q) options
A.7.1 Option Q1: Quantification using external standards in solvent
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
A.7.2.1 Principle
A.7.2.2 Procedure
75 A.7.2.3 Calculation
A.7.3 Option Q3: Quantification using a procedural internal standard and standards in solvent
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
A.7.4.1 Principle
A.7.4.2 Procedure
A.7.4.3 Calculation
76 A.7.5 Option Q5: Quantification using a procedural internal standard and standards in matrix or isotope-labelled internal standards
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
A.7.6.1 Principle
77 A.7.6.2 Procedure
A.7.6.3 Calculation
A.7.7 Option Q7: Quantification by calibration of the entire procedure
A.7.7.1 Principle
A.7.7.2 Procedure
A.7.7.3 Calculation
78 Annex B (informative)Complementary information
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
79 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
80 Annex C (informative)Abbreviations

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BS EN 15662:2018
$215.11