Overview
ISO/TS 16465:2024 specifies validated laboratory methods for the quantitative determination of phthalates in vegetable oils using gas chromatography–mass spectrometry (GC‑MS). The Technical Specification is published by ISO and is split into two parts:
- Part A – targeted determination of di‑2‑ethylhexyl phthalate (DEHP).
- Part B – determination of eight phthalates: DMP, DEP, DIBP, DBP, BBP, DEHP, DINP, DIDP.
Both methods apply to all vegetable oils (crude, refined and virgin) and cover sample preparation, extraction, clean‑up, instrumental analysis, calibration and method performance characteristics.
Key topics and technical requirements
- Analytical principle: extraction with acetonitrile, dispersive solid‑phase extraction (dispersive‑SPE) clean‑up using PSA (primary secondary amine) and C18 sorbents, concentration of the extract and GC‑MS analysis (SIM mode).
- Target analytes: DEHP (Part A) and a panel of eight phthalates (Part B): DMP, DEP, DIBP, DBP, BBP, DEHP, DINP, DIDP.
- Reagents and standards: toluene, acetonitrile, n‑hexane, n‑dodecane, PSA and C18 sorbents; use of a deuterated internal standard (DEHP‑d4) and a defined calibration series.
- Instrumentation: capillary GC with MS detector (electron ionization at 70 eV), single ion monitoring (SIM), and high‑temperature capillary columns suitable for phthalate analysis.
- Apparatus and cleanliness: strict glassware cleaning (e.g., 550 °C for 6 h), centrifugation, micro‑syringes and optional automated evaporator for concentration steps.
- Quality and validation: procedures for calibration curves, quantitative calculation, and documented precision data (interlaboratory tests, repeatability and reproducibility).
- Sampling and sample handling: analyse aliquots supplied in glass bottles; recommended lid contact materials include PTFE, aluminium or rubber - avoid plastic contact materials.
Applications and users
ISO/TS 16465:2024 supports:
- Food and edible oil testing laboratories performing compliance and contamination testing for phthalates in vegetable oils.
- Oil producers and refiners for in‑house quality control and supplier verification.
- Regulatory authorities and food safety agencies monitoring phthalate residues in edible fats and oils.
- Research institutions studying phthalate migration, exposure or processing impacts.
- Contract testing and environmental labs when assessing phthalate contamination from packaging or processing.
Keywords: ISO/TS 16465:2024, phthalates in vegetable oils, DEHP determination, GC‑MS phthalate analysis, dispersive solid‑phase extraction, PSA C18 cleanup.
Related standards
- ISO 661 - Preparation of test sample for animal and vegetable fats and oils (normative reference).
- Recommended sampling guidance referenced: ISO 5555 (sampling of vegetable oils).