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BS EN 15662:2018 – TC:2020 Edition

BS EN 15662:2018 – TC:2020 Edition

$280.87

Tracked Changes. 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

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BSI 2020 0
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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, 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 FprCEN/TR 17063. Guidelines for calibration are outlined in FprCEN/TS 17061.

PDF Catalog

PDF Pages PDF Title
1 compares BS EN 15662:2018
2 TRACKED CHANGES
Text example 1 — indicates added text (in green)
166 undefined
170 1 Scope
2 Normative references
3 Principle
4 Preparation and storage of the samples
4.1 General
4.2 Laboratory sample
171 4.3 Partly-prepared test sample
4.4 Test sample
4.5 Test portion
5 Procedure
181 6 Evaluation of results
6.1 Identification and quantification
6.2 Calibration
6.3 Calculation of residue concentration
182 6.4 Validity of the method
188 7 Confirmatory tests
8 Precision
9 Test report
189 Annex A (informative)Description of modules
A.1 Reagents used in all extraction (E) and clean-up (C) and stabilization (S) modules
192 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
193 A.3.1.2 Procedure
A.3.1.3 Calculation
194 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
195 A.3.2.2 Procedure
A.3.2.3 Calculation
196 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
197 A.3.3.2 Procedure
A.3.3.3 Calculation
198 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
199 A.3.4.2 Procedure
A.3.4.3 Calculation
200 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
201 A.3.5.2 Procedure
A.3.5.3 Calculation
202 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
203 A.3.6.2 Procedure
A.3.6.3 Calculation
204 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
205 A.3.7.2 Procedure
A.3.7.3 Calculation
206 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
207 A.3.8.2 Procedure
A.3.8.3 Calculation
208 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
209 A.3.9.2 Procedure
210 A.3.9.3 Calculation
A.3.9.4 Flowchart of module E9
211 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
212 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
213 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
214 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
215 A.4.4.2 Procedure
A.4.4.3 Calculation
216 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
217 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
218 A.4.6.2 Procedure
A.4.6.3 Calculation
219 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
220 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
223 A.6.1.5 Procedural remarks
224 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
228 A.6.2.5 Procedural remarks
229 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
231 A.6.3.5 Procedural remarks
232 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
233 A.6.4.4 Examples of suitable conditions
234 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
235 A.6.5.3 Apparatus
A.6.5.4 Examples of suitable conditions
236 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
238 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
239 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
240 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
241 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
242 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
243 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
244 Annex C (informative)Abbreviations

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BS EN 15662:2018 - TC
$280.87