Multiresidue mycotoxin analysis in wheat, barley, oats, rye and maize grain by high-performance liquid chromatography-tandem mass spectrometry
Bibliographic record
Abstract
A method has been developed for the simultaneous analysis of 22 mycotoxins in wheat, barley, oats, rye and maize grain. Analysis is carried out with liquid chromatography-electrospray ionisation tandem mass spectrometry. The compounds included in this analysis are aflatoxins, sterigmatocystin, cyclopiazonic acid, tricothecenes, ochratoxin A, fumonisins, zearalonone, and ergot alkaloids. Sample extraction (2 g) with acetonitrile:water (8 ml, 80:20) was carried out for 2 min using a commercial sample preparation apparatus (Stomacher®). The extract was then centrifuged, filtered and analysed. Extraction of fumonisins from maize (2 g) was optimised by first extracting the maize with acetonitrile: water (5 ml, 80:20) followed by the addition of water (3 ml), which permitted extraction of the 22 mycotoxins, including the fumonisins. Chromatography was carried out with a minicolumn (7.5×2.1 mm, 5 µm) (5 µl sample injection) and in 11 min, including column reconditioning. Analysis was carried out with 2 MRM transitions for the precursor ions. All method detection limits were below current maximum Canadian residue limits. Matrix effects for each compound in each of the 5 matrices were estimated and ranged from 70 to 149%, but most were 100±10%. Accuracy, repeatability and ruggedness were established. Proficiency samples from FERA (Food and Environment Research Agency, Sand Hutton, York, UK) were tested and are reported. Finally, 100 field samples of the various grains were tested with this method and are reported with the observation of numerous mycotoxins in all matrices, including ergotamine in winter wheat.
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How this classification was reachedexpand
Full frame machine prediction
Teacher imitationNot calibrated prevalence, not ground truth. Human validation pending. The Gemma side is a direct model label for every work in the frame, read from the title-only record. The Codex side is a classifier learned from the 10,348 direct Codex labels and calibrated to design-weighted sample rates; fields without enough sample support carry no Codex call. Candidate is the union of the two sides; consensus is their intersection. These outputs are machine_predicted_unvalidated and are not human labels.
Distilled classifier scores by category (both heads)
| Category | Codex | Gemma |
|---|---|---|
| Metaresearch | 0.000 | 0.000 |
| Meta-epidemiology (narrow) | 0.001 | 0.000 |
| Meta-epidemiology (broad) | 0.001 | 0.000 |
| Bibliometrics | 0.001 | 0.001 |
| Science and technology studies | 0.000 | 0.000 |
| Scholarly communication | 0.001 | 0.000 |
| Open science | 0.000 | 0.000 |
| Research integrity | 0.001 | 0.000 |
| Insufficient payload (model declined to judge) | 0.000 | 0.000 |
Machine scores (provisional)
The two teacher heads of the student model, read on this work. A score orders the frame for review; it never asserts a category, and the validation status ships verbatim with every row.
Baseline scores from an immature model (maturity gate not passed, 7 training rounds). Scores rank; they never assert a category.
score_only:v0-immature-baseline · verbatim from the scoring run: score_only means the number may rank works, and no category label ships from itClassification
machine, unvalidatedMachine predicted; a candidate call from one source (direct Gemma or distilled Codex), not a consensus.
How this classification was reached, model by model and score by score, is at the end of the page under "How this classification was reached".