Development and Validation of a GC–MS Method Based on Solid-Phase Extraction and Derivatization for Analysis of Free and Glucuronide-Conjugated Bisphenol F in Biological Samples
Bibliographic record
Abstract
BACKGROUND: As one of the speculated bisphenols to replace bisphenol A (BPA), bisphenol F (BPF), naturally present in mustard, is structurally similar to BPA and may have similar estrogenic activity, but information on its toxicity is very limited compared to BPA. OBJECTIVE: In order to support the toxicology study of BPF at Heath Canada, a GC-MS method based on solid-phase extraction (SPE) and derivatization was developed for analysis of BPF in liver samples. METHODS: Samples were treated with β-glucuronidase to convert BPF glucuronide to free BPF for analysis of total BPF. RESULTS: The method was validated for free BPF at different spiking levels, and recoveries ranged from 90-97.5% with RSDs from 0.11-5.54%. The method was also validated for glucuronide-conjugated BPF at different spiking levels of BPF mono-β-D-glucuronide: recoveries ranged from 72.3-93.3% with RSDs from 1.7-8.94%. The method was used to analyze 60 liver tissue samples from rats dosed with BPF at different levels in a toxicology study. Free and glucuronide-conjugated BPF were not detected in any of the control samples, which were not dosed with BPF (average method detection limit: 0.31 ng/g) but detected in all the other liver tissue samples with levels increasing at higher doses. The percentage of glucuronide-conjugated BPF in total BPF varied among the liver samples, from as low as 9.8% to as high as 77.9%, indicating the importance of analyzing biological samples for BPF in both free and conjugated forms for total exposure. CONCLUSION: A GC-MS method based on solid-phase extraction (SPE) and derivatization was developed for analysis of both free and glucuronide-conjugated BPF in liver samples. This method was validated not only for free BPF, but also for mono-β-D-glucuronide-conjugated BPF for the first time to confirm the efficiency of the deconjugation procedure with enzyme. HIGHLIGHTS: This method can be adapted and applied for analysis of free and glucuronide-conjugated BPF in other biological samples with appropriate validation in target sample matrixes.
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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 | 0.002 | 0.002 |
| Meta-epidemiology (narrow) | 0.002 | 0.001 |
| Meta-epidemiology (broad) | 0.001 | 0.001 |
| Bibliometrics | 0.002 | 0.001 |
| Science and technology studies | 0.001 | 0.001 |
| Scholarly communication | 0.001 | 0.001 |
| Open science | 0.001 | 0.001 |
| Research integrity | 0.002 | 0.001 |
| Insufficient payload (model declined to judge) | 0.001 | 0.001 |
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".