Rapid non-separative determination of prevailing organophosphate flame retardants metabolites in urine by means of a restricted access material coupled to tandem mass spectrometry
Bibliographic record
Abstract
• BDCPP and DPhP determination in human urine in less than 5 min. • The combination of RAM and MS/MS avoid the need for a chromatographic separation. • Validated with certified urine samples (86%-108% accuracy). Organophosphate flame retardants (OPFRs) are used to reduce the flammability of various materials. Among these compounds, triphenyl phosphate (TPhP) and tris(1,3-dichloro-2-propyl) phosphate (TDCIPP) are prominent OPFRs associated with reproductive and endocrine-disrupting effects. Monitoring their urinary metabolites, diphenyl phosphate (DPhP) and bis(1,3-dichloro-2-propyl) phosphate (BDCPP), are crucial for assessing bioaccumulation, toxicity, and exposure. This study presents a novel, non-separative analytical method combining restricted access material (RAM) with tandem mass spectrometry (MS/MS), eliminating the need for chromatographic separation. This innovation significantly reduces total analysis time down to less than five minutes per sample (12 samples per hour), compared to up to 37 min (only one sample per hour) required by state-of-the-art separative methods. The method achieves sub-ppb limits of quantification (LOQ ≤ 0.1 ng mL −1 ) that are equal or better than those achieved by separative methodologies. Matrix effects were minimized (≃20 %) with a conventional clean-up pretreatment based on SPE. The whole methodology was validated by analyzing certified urine samples provided by Centre de toxicologie du Québec and applied to the analysis of real urine samples from non-exposed individuals. The accuracy (86–108 %), precision (RSD < 20 %) and high recovery (98–109 %) confirm the robustness and suitability of this method in routine laboratory applications. This is the first report, to the best of our knowledge, to fully integrate RAM with direct MS/MS analysis for most prominent urinary OPFR metabolites without chromatographic separation. This methodological advance offers substantial advantages in speed, simplicity, and adaptability to high-throughput biomonitoring studies, setting a new benchmark for the determination of DPhP and BDCPP in human urine.
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How this classification was reachedexpand
Full frame distilled prediction
Teacher imitationNot calibrated prevalence, not ground truth. Human validation pending. Learned from the 10,348 direct Codex labels and 10,348 direct Gemma labels. Candidate is the union of thresholded teacher heads; consensus is their intersection. These outputs are machine_predicted_unvalidated and are not human labels or direct frontier model labels.
Codex and Gemma teacher scores by category
| Category | Codex | Gemma |
|---|---|---|
| Metaresearch | 0.000 | 0.000 |
| Meta-epidemiology (narrow) | 0.000 | 0.000 |
| Meta-epidemiology (broad) | 0.000 | 0.000 |
| Bibliometrics | 0.000 | 0.001 |
| Science and technology studies | 0.000 | 0.000 |
| Scholarly communication | 0.000 | 0.000 |
| Open science | 0.000 | 0.000 |
| Research integrity | 0.000 | 0.000 |
| Insufficient payload (model declined to judge) | 0.003 | 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 teacher head, 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".