Abstract

The principles and application of established and newer methods for the quantitative and semi-quantitative determination of ergot alkaloids in food, feed, plant materials and animal tissues are reviewed. The techniques of sampling, extraction, clean-up, detection, quantification and validation are described. The major procedures for ergot alkaloid analysis comprise liquid chromatography with tandem mass spectrometry (LC-MS/MS) and liquid chromatography with fluorescence detection (LC-FLD). Other methods based on immunoassays are under development and variations of these and minor techniques are available for specific purposes.

Highlights

  • solid-phase extraction (SPE) clean-up based on various different chemistries can be applied to the clean-up of ergot alkaloids (EA) extracts, including basic alumina cartridges, C18 reversed phase, Hydrophilic-Lipophilic Balance (HLB), strong cation exchange (SCX), mixed-mode cation exchange (MCX) cartridges and immunoaffinity methods using immunoaffinity columns (IAC)

  • Antibodies are raised that bind to the lysergic acid ring structure, many peptide alkaloids have large groups attached to the lysergic acid which hinder the antibody binding and are not amenable to Enzyme Linked Immunosorbent Assays (ELISA)

  • The method is intended for use in cereal conveyor belt systems at an industrial level and has identified a sclerotia content of 0.02%, which is below the European Commission limits of 0.1% for feedstuffs containing unground cereals, and 0.05% in “intervention” cereals destined for human consumption

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Summary

Ergot Alkaloids

The analysis of ergot alkaloids (EA) is of considerable importance, and a substantial topic because the alkaloids are encountered in many different situations that affect humans and animals, and they are found in many different matrices. Developments in instrumental techniques have given us the ability to separate and measure individual ergot compounds and their isomers, and this in turn has allowed the possibility of monitoring and regulating the contamination of cereal based foods. There is a requirement to measure EA in ergot sclerotia, infected cereals, Toxins 2015, 7 forage grasses, processed foods, pharmaceutical preparations, illicit preparations, and body fluids and organs. Chemical analysis today usually follows a distinct pathway of careful sampling and homogenisation, extraction of the analyte, separation of the analyte from co-extracted materials (clean-up), detection and quantification. Examples of these procedure are provided in the following paragraphs.

Lysergic Acid Amides
Ergopeptines
Stability
Sampling
Extraction
Clean-up
Capillary Electrophoresis
Gas Chromatography-Mass Spectrometry
Liquid Chromatography
Ultraviolet and Fluorescence Detection
Introduction
Matrix Effects
Identification and Quantification
Multiresidue Mycotoxin Screening Methods
Immunological Methods
10. Other Spectroscopic Methods
11. Other Methods
12. Method Performance
13. Method Validation
14. Specific Applications
14.2. Other EA
14.3. Forensic Analysis and Body Tissues
14.4. Pharmaceutical Formulations
Findings
15. Conclusions

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