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BS EN 17425:2021

$189.07

Foodstuffs. Determination of ergot alkaloids in cereals and cereal products by dSPE clean-up and HPLC-MS/MS

Published By Publication Date Number of Pages
BSI 2021 48
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This document describes a method for the determination of the sum of six ergot alkaloids (ergocornine, ergometrine, ergocristine, ergotamine, ergosine and ergocryptine) and their -inine epimer pairs by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) after clean-up by dispersive solid phase extraction (dSPE).

The method has been validated in the range 13,2 µg/kg to 168 µg/kg for the sum of the twelve ergot alkaloids, in rye flour, rye bread and cereal products (breakfast cereal, infant breakfast cereal, and crispbread) that contained rye as an ingredient, as well as seeded wholemeal flour and a barley and rye flour mixture.

Method performance was satisfactory in the range 24,1 µg/kg to 168 µg/kg, however at lower concentrations RSDR values were greater than 44 %, and HorRat values exceeded 2,0, indicating the method may not be fully suitable at concentrations below 24 µg/kg for sum of ergot alkaloids, although it is suitable for screening at these concentrations.

PDF Catalog

PDF Pages PDF Title
2 undefined
8 1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Reagents
10 6 Apparatus and equipment
11 7 Procedure
7.1 Preparation of the test sample
12 7.2 Extraction of ergot alkaloids
7.2.1 Precautions
7.2.2 Test sample
7.2.3 Spiking procedure
7.2.4 Sample extraction
7.2.5 Clean-up
8 LC-MS/MS analysis
8.1 General
13 8.2 Batch composition and analytical sequence
8.3 Identification
8.4 Calibration
9 Calculation
9.1 Calculation of individual ergot alkaloid concentration
14 9.2 Calculation of ergot alkaloid sum concentration
10 Precision
10.1 General
10.2 Repeatability
10.3 Reproducibility
15 11 Test report
16 Annex A (informative)Example conditions for suitable LC-MS/MS systems
A.1 System settings for Waters® Xevo® TQ-S Mass Spectrometer
A.1.1 Settings for chromatography
17 A.1.2 Detector parameters
19 A.2 System settings for Micromass® Quattro Ultima Pt Mass Spectrometer
A.2.1 Settings for chromatography
20 A.2.2 Detector parameters
21 A.3 System settings for SCIEX API 5500 Mass Spectrometer
A.3.1 Settings for chromatography
22 A.3.2 Detector parameters
24 A.4 Other LC conditions
25 Annex B (informative)Typical chromatograms
31 Annex C (informative)Precision data
45 Annex D (informative)Data comparison
BS EN 17425:2021
$189.07