Determination of Pyrrolizidine Alkaloids in Tea and Herbal Infusions by LC-MS/MS.
5 affiliations
- 1Associate Laboratory i4HB-Institute for Health and Bioeconomy, CESPU University, 4585-116 Gandra, Portugal.
- 2UCIBIO-Research Unit on Applied Molecular Biosciences, Toxicologic Pathology Research Laboratory, CESPU University, 4585-116 Gandra, Portugal.
- 3LSRE-LCM, ALiCE, Faculty of Engineering, University of Porto, 4200-465 Porto, Portugal.
- 4UCIBIO-Research Unit on Applied Molecular Biosciences, Translational Toxicology Research Laboratory, CESPU University, 4585-116 Gandra, Portugal.
- 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 -