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 |
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 |
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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 |