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BS EN 17280:2019

BS EN 17280:2019

$198.66

Foodstuffs. Determination of zearalenone and trichothecenes including deoxynivalenol and its acetylated derivatives (3-acetyl-deoxynivalenol and 15-acetyl-deoxynivalenol), nivalenol T-2 toxin and HT-2 toxin in cereals and cereal products by LC-MS/MS

Published By Publication Date Number of Pages
BSI 2019 52
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This document specifies a procedure for the determination of nivalenol (NIV), deoxynivalenol (DON) and its acetyl derivatives (3-acetyl-DON and 15-acetyl-DON), HT-2 and T-2 toxins (HT-2 and T-2) and zearalenone (ZEN) in cereals and cereal products by high performance liquid chromatography (HPLC) coupled with tandem mass spectrometry (MS/MS) after clean-up by solid phase extraction (SPE).

The method has been validated with samples of wheat, wheat flour, and wheat crackers. The wheat and the wheat flour were prepared from a mixture of wheat and fungi infected wheat kernels. The wheat crackers were baked from wheat flour and water spiked with the target mycotoxins.

Validation levels for NIV ranged from 27,7 ?g/kg to 378 ?g/kg.

Validation levels for DON ranged from 234 ?g/kg to 2420 ?g/kg.

Validation levels for 3-acetyl-DON ranged from 18,5 ?g/kg to 137 ?g/kg.

Validation levels for 15-acetyl-DON ranged from 11,4 ?g/kg to 142 ?g/kg.

Validation levels for HT-2 ranged from 6,6 ?g/kg to 134 ?g/kg.

Validation levels for T-2 ranged from 2,1 ?g/kg to 37,6 ?g/kg.

Validation levels for ZEN ranged from 31,6 ?g/kg to 230 ?g/kg.

Laboratory experiences have shown that this method is also applicable to barley and oat flour, and rye based crackers [5], however, this has not been validated in a collaborative study.

PDF Catalog

PDF Pages PDF Title
2 undefined
7 1 Scope
2 Normative references
3 Terms and definitions
4 Principle
8 5 Reagents
10 6 Apparatus and equipment
11 7 Procedure
7.1 Preparation of the test sample
7.2 Extraction
7.3 Solid phase extraction clean up
7.4 Preparation of the sample test solution
7.5 Spiking procedure
12 7.6 LC-MS/MS analysis
7.6.1 General
7.6.2 Injection sequence
7.7 Identification
7.8 Calibration
13 8 Calculation
9 Precision
9.1 General
9.2 Repeatability
9.3 Reproducibility
17 10 Test report
18 Annex A (informative)Typical chromatograms
A.1 Example chromatogram using the settings according to B.1
19 A.2 Example chromatogram using the settings according to B.2
20 Annex B (informative)Example conditions for suitable LC-MS/MS systems
B.1 System Settings for API SCIEX 5000™,
B.1.1 Settings for chromatography
21 B.1.2 Detector parameters
22 B.2 System settings for Thermo Q-Exactive™,
B.2.1 Settings for chromatography
23 B.2.2 Detector Parameters
26 Annex C (informative)Additional examples for separation between 3-AcDON and 15-AcDON
C.1 Settings for AccucoreTM C18 (Thermo Scientific)
27 C.2 Settings for Kinetex® C18 (Phenomenex)4
C.3 Settings for Kinetex® PFP (Phenomenex)
29 Annex D (informative)Precision data

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BS EN 17280:2019
$198.66