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Peer-reviewedCC BYFoods (Basel, Switzerland)

Determination of Pyrrolizidine Alkaloids in Tea and Herbal Infusions by LC-MS/MS.

5 affiliations
  1. 1Associate Laboratory i4HB-Institute for Health and Bioeconomy, CESPU University, 4585-116 Gandra, Portugal.
  2. 2UCIBIO-Research Unit on Applied Molecular Biosciences, Toxicologic Pathology Research Laboratory, CESPU University, 4585-116 Gandra, Portugal.
  3. 3LSRE-LCM, ALiCE, Faculty of Engineering, University of Porto, 4200-465 Porto, Portugal.
  4. 4UCIBIO-Research Unit on Applied Molecular Biosciences, Translational Toxicology Research Laboratory, CESPU University, 4585-116 Gandra, Portugal.
  5. 5UNIPRO-Oral Pathology and Rehabilitation Research Unit, CESPU University, 4585-116 Gandra, Portugal.

Abstract

Pyrrolizidine alkaloids (PAs) and N-oxides (PANOs) are food-safety hazards subject to regulatory limits, and their occurrence in teas and herbal infusions (THI) represents a dietary route. This study aimed to develop and validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determining five PAs and their PANOs in THI. Samples were extracted using hot acidified water to enhance PAs and PANOs extraction and subjected to solid-phase extraction (SPE) for clean-up and analyte preconcentration. Chromatographic separation was performed on a Luna® PFP (2) 3 µm 100 Å column using a gradient of 10 mM ammonium formate with 0.1% formic acid in water, ethanol, and methanol. The method was validated according to international guidelines, achieving detection and quantification limits of 0.41-6.60 ng/g and 1.25-20.0 ng/g. It was applied to 53 THI samples from five European countries, primarily from Portugal as a pilot monitoring study. N-oxides were the predominant form, with senecionine-N-oxide, heliotrine-N-oxide, and retrorsine-N-oxide most frequently detected in Portuguese-marketed products. The total target PA/PANO content was approximately twofold higher in herbal infusions than in teas, with chamomile showing the highest levels, followed by lemon verbena. The validated method provides a sensitive and suitable tool for preliminary assessment of PAs and PANOs in THI.

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BibTeX
@article{sousa2026determination,
  title = {{Determination of Pyrrolizidine Alkaloids in Tea and Herbal Infusions by LC-MS/MS.}},
  author = {Ana Catarina Sousa and Daniela Pereira and Ana R L Ribeiro and Virgínia M F Gonçalves and Inês Pádua and Cláudia Ribeiro and Sandra Leal},
  journal = {Foods (Basel, Switzerland)},
  year = {2026},
  month = oct,
  doi = {10.3390/foods15203598},
  url = {https://europepmc.org/article/MED/42940235},
  note = {CC BY},
}
RIS
TY  - JOUR
TI  - Determination of Pyrrolizidine Alkaloids in Tea and Herbal Infusions by LC-MS/MS.
AU  - Ana Catarina Sousa
AU  - Daniela Pereira
AU  - Ana R L Ribeiro
AU  - Virgínia M F Gonçalves
AU  - Inês Pádua
AU  - Cláudia Ribeiro
AU  - Sandra Leal
PY  - 2026
DA  - 2026/10/10
JO  - Foods (Basel, Switzerland)
DO  - 10.3390/foods15203598
UR  - https://europepmc.org/article/MED/42940235
AB  - Pyrrolizidine alkaloids (PAs) and N-oxides (PANOs) are food-safety hazards subject to regulatory limits, and their occurrence in teas and herbal infusions (THI) represents a dietary route. This study aimed to develop and validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determining five PAs and their PANOs in THI. Samples were extracted using hot acidified water to enhance PAs and PANOs extraction and subjected to solid-phase extraction (SPE) for clean-up and analyte preconcentration. Chromatographic separation was performed on a Luna® PFP (2) 3 µm 100 Å column using a gradient of 10 mM ammonium formate with 0.1% formic acid in water, ethanol, and methanol. The method was validated according to international guidelines, achieving detection and quantification limits of 0.41-6.60 ng/g and 1.25-20.0 ng/g. It was applied to 53 THI samples from five European countries, primarily from Portugal as a pilot monitoring study. N-oxides were the predominant form, with senecionine-N-oxide, heliotrine-N-oxide, and retrorsine-N-oxide most frequently detected in Portuguese-marketed products. The total target PA/PANO content was approximately twofold higher in herbal infusions than in teas, with chamomile showing the highest levels, followed by lemon verbena. The validated method provides a sensitive and suitable tool for preliminary assessment of PAs and PANOs in THI.
SN  - 2304-8158
ER  -