Quantitative Analysis of Pyrrolizidine Alkaloids in Food Matrices and Plant-Derived Samples Using UHPLC—MS/MS

Pyrrolizidine alkaloids (PAs) are a class of nitrogen-containing basic organic compounds that are frequently detected in foods and herbal medicines. Owing to their potential hepatotoxic, genotoxic, and carcinogenic properties, PAs have become a significant focus for monitoring global food safety. In...

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Main Authors: Runfeng Lin, Jing Peng, Yingjie Zhu, Suhe Dong, Xin Jiang, Danning Shen, Jiaxin Li, Peihong Zhu, Jie Mao, Na Wang, Kun He
Format: Article
Language:English
Published: MDPI AG 2025-03-01
Series:Foods
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Online Access:https://www.mdpi.com/2304-8158/14/7/1147
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author Runfeng Lin
Jing Peng
Yingjie Zhu
Suhe Dong
Xin Jiang
Danning Shen
Jiaxin Li
Peihong Zhu
Jie Mao
Na Wang
Kun He
author_facet Runfeng Lin
Jing Peng
Yingjie Zhu
Suhe Dong
Xin Jiang
Danning Shen
Jiaxin Li
Peihong Zhu
Jie Mao
Na Wang
Kun He
author_sort Runfeng Lin
collection DOAJ
description Pyrrolizidine alkaloids (PAs) are a class of nitrogen-containing basic organic compounds that are frequently detected in foods and herbal medicines. Owing to their potential hepatotoxic, genotoxic, and carcinogenic properties, PAs have become a significant focus for monitoring global food safety. In this study, an ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method was developed for the detection and analysis of three foods (tea, honey, and milk) susceptible to PA contamination. This optimized method effectively separated and detected three types of PAs, namely, three pairs of isomers and two pairs of chiral compounds. The limits of detection (LODs) and limits of quantification (LOQs) were determined to be 0.015–0.75 and 0.05–2.5 µg/kg, respectively, with the relative standard deviations (RSDs) of both the interday and intraday precisions remaining below 15%. The average PA recoveries from the honey, milk, and tea matrices fell within the ranges of 64.5–103.4, 65.2–112.2, and 67.6–107.6%, respectively. This method was also applied to 77 samples collected from 33 prefecture-level cities across 16 provinces and included 40 tea, 6 milk, 8 honey, 14 spice, and 9 herbal medicine samples. At least one PA was detected in twenty-three of the samples, with herbal medicines exhibiting the highest total PA content. The obtained results indicate that the developed method demonstrated good repeatability and stability in the detection and quantitative analyses of PAs in food- and plant-derived samples. This method is therefore expected to provide reliable technical support for food safety risk monitoring.
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spelling doaj-art-c9a36dbc41094960beeef6e94ea66e562025-08-20T02:17:00ZengMDPI AGFoods2304-81582025-03-01147114710.3390/foods14071147Quantitative Analysis of Pyrrolizidine Alkaloids in Food Matrices and Plant-Derived Samples Using UHPLC—MS/MSRunfeng Lin0Jing Peng1Yingjie Zhu2Suhe Dong3Xin Jiang4Danning Shen5Jiaxin Li6Peihong Zhu7Jie Mao8Na Wang9Kun He10National Center of Biomedical Analysis, Beijing 100850, ChinaNational Center of Biomedical Analysis, Beijing 100850, ChinaNational Center of Biomedical Analysis, Beijing 100850, ChinaNational Center of Biomedical Analysis, Beijing 100850, ChinaNational Center of Biomedical Analysis, Beijing 100850, ChinaNational Center of Biomedical Analysis, Beijing 100850, ChinaNational Center of Biomedical Analysis, Beijing 100850, ChinaNational Center of Biomedical Analysis, Beijing 100850, ChinaNational Center of Biomedical Analysis, Beijing 100850, ChinaNational Center of Biomedical Analysis, Beijing 100850, ChinaNational Center of Biomedical Analysis, Beijing 100850, ChinaPyrrolizidine alkaloids (PAs) are a class of nitrogen-containing basic organic compounds that are frequently detected in foods and herbal medicines. Owing to their potential hepatotoxic, genotoxic, and carcinogenic properties, PAs have become a significant focus for monitoring global food safety. In this study, an ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method was developed for the detection and analysis of three foods (tea, honey, and milk) susceptible to PA contamination. This optimized method effectively separated and detected three types of PAs, namely, three pairs of isomers and two pairs of chiral compounds. The limits of detection (LODs) and limits of quantification (LOQs) were determined to be 0.015–0.75 and 0.05–2.5 µg/kg, respectively, with the relative standard deviations (RSDs) of both the interday and intraday precisions remaining below 15%. The average PA recoveries from the honey, milk, and tea matrices fell within the ranges of 64.5–103.4, 65.2–112.2, and 67.6–107.6%, respectively. This method was also applied to 77 samples collected from 33 prefecture-level cities across 16 provinces and included 40 tea, 6 milk, 8 honey, 14 spice, and 9 herbal medicine samples. At least one PA was detected in twenty-three of the samples, with herbal medicines exhibiting the highest total PA content. The obtained results indicate that the developed method demonstrated good repeatability and stability in the detection and quantitative analyses of PAs in food- and plant-derived samples. This method is therefore expected to provide reliable technical support for food safety risk monitoring.https://www.mdpi.com/2304-8158/14/7/1147pyrrolizidine alkaloidsUHPLC—MS/MShoneyteamilkfood safety
spellingShingle Runfeng Lin
Jing Peng
Yingjie Zhu
Suhe Dong
Xin Jiang
Danning Shen
Jiaxin Li
Peihong Zhu
Jie Mao
Na Wang
Kun He
Quantitative Analysis of Pyrrolizidine Alkaloids in Food Matrices and Plant-Derived Samples Using UHPLC—MS/MS
Foods
pyrrolizidine alkaloids
UHPLC—MS/MS
honey
tea
milk
food safety
title Quantitative Analysis of Pyrrolizidine Alkaloids in Food Matrices and Plant-Derived Samples Using UHPLC—MS/MS
title_full Quantitative Analysis of Pyrrolizidine Alkaloids in Food Matrices and Plant-Derived Samples Using UHPLC—MS/MS
title_fullStr Quantitative Analysis of Pyrrolizidine Alkaloids in Food Matrices and Plant-Derived Samples Using UHPLC—MS/MS
title_full_unstemmed Quantitative Analysis of Pyrrolizidine Alkaloids in Food Matrices and Plant-Derived Samples Using UHPLC—MS/MS
title_short Quantitative Analysis of Pyrrolizidine Alkaloids in Food Matrices and Plant-Derived Samples Using UHPLC—MS/MS
title_sort quantitative analysis of pyrrolizidine alkaloids in food matrices and plant derived samples using uhplc ms ms
topic pyrrolizidine alkaloids
UHPLC—MS/MS
honey
tea
milk
food safety
url https://www.mdpi.com/2304-8158/14/7/1147
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