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BSI 16/30337114 DC:2016 Edition

BSI 16/30337114 DC:2016 Edition

$13.70

BS EN 16987. Foodstuffs. Determination of acrylamide in coffee and coffee products by HPLC-MS/MS and GC-MS

Published By Publication Date Number of Pages
BSI 2016 25
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PDF Catalog

PDF Pages PDF Title
4 Contents Page
5 European foreword
6 Introduction
7 1 Scope
2 Normative references
3 Principle
4 Reagents
9 5 Apparatus
10 6 Procedure
6.1 General
6.2 Preparation of the sample extract
6.3 Clean-up of the extracts
6.3.1 Carrez precipitation
6.3.2 Solid phase extraction
11 6.4 HPLC-MS/MS measurement
6.4.1 High performance liquid chromatography (HPLC)
6.4.2 Identification and quantification by mass spectrometry (HPLC-MS/MS)
Table 1 — Mass spectrometric transitions used for the identification and quantification of acrylamide
12 6.5 Measurement with GC-MS
6.5.1 Derivatisation and sample preparation for gas chromatography
6.5.2 Gas chromatography
6.5.3 Identification and quantification by mass spectrometry
13 Table 2 — Observed ions
7 Calibration
7.1 General advice
7.2 Determination of linearity and definition of the working range
7.3 Calibration with internal standard
7.4 Determination of the laboratory specific recovery
14 8 Evaluation
8.1 Criteria for identification
8.2 Calculation and final results
9 Precision data
9.1 General
9.2 Repeatability
15 9.3 Reproducibility
Table 3 — Precision data for the determination of acrylamide in coffee
9.4 Recovery
10 Measurement uncertainty
11 Test report
16 Annex A (informative) Performance characteristics
Table A.1 — Inter-laboratory study results (for both HPLC-and GC variants)0F )
17 Annex B (informative) Examples of absorber materials
Table B.1 — Examples of suitable sorbents for the SPE clean-up (HPLC and GC, see 6.3)
Table B.2 — Examples of suitable sorbents for the SPE clean-up of the GC extract (see 6.5.1)
18 Annex C (informative) Examples for recommended columns and analysis conditions
C.1 Generally suitable chromatographic columns
Table C.1 — Analytical conditions for selected HPLC columns
Table C.2 — GC capillary columns
19 C.2 Example method and approximate retention time for HPLC-MS/MS
C.2.1 Example A
Table C.3 — Chromatographic conditions for example A
C.2.2 Example B
Table C.4 — Chromatographic conditions for example B
C.3 Example of suitable conditions and approximate retention time for GC-MS analysis
20 Table C.5 — GC method: Example of suitable conditions and approximate retention time for GC-MS
21 C.4 Example chromatograms for HPLC-MS/MS
Figure C.1 — D3-acrylamide
22 Figure C.2 — Acrylamide, native
23 C.5 Example of chromatogram for GC-MS
Figure C.3 — Total ion chromatogram (scan mode)
24 Figure C.4 — Extracted ion, mass 149 (quantifier ion)
Figure C.5 — Extracted ion, mass 106 (qualifier ion)
25 Bibliography

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BSI 16/30337114 DC
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