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Determination of 35 pyrrolizidine alkaloids in dried tea by ultra-high performance liquid chromatography- triple quadrupole mass spectrometry
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Lu DONG1, Xiaolin ZHANG2, Chen YANG1, Jingyan ZHAO1, Xuemei WANG1, Yingqian CHU2, Xuehua LI1, *
Chinese Journal of Chromatography | 2025, 43(12) : 1342 - 1353
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Chinese Journal of Chromatography | 2025, 43(12): 1342-1353
• Articles •
Determination of 35 pyrrolizidine alkaloids in dried tea by ultra-high performance liquid chromatography- triple quadrupole mass spectrometry
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Lu DONG1, Xiaolin ZHANG2, Chen YANG1, Jingyan ZHAO1, Xuemei WANG1, Yingqian CHU2, Xuehua LI1, *
Affiliations
  • 1. Key Laboratory of Industrial Ecology and Environmental Engineering,School of Environment,Dalian University of Technology,Dalian 116024,China
  • 2. Technology Center of Dalian Customs District,Dalian 116001,China
Published: 2025-12-08 doi: 10.3724/SP.J.1123.2025.01020
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Pyrrolizidine alkaloids (PAs) are natural toxins widely distributed in plants, which naturally occur in about 3% of the world’s flowering plants. To date, more than 660 PAs and their nitrogen oxides have been identified in over 6 000 plants. Some PAs are hepatotoxic, genotoxic and tumorigenic, posing significant health risks to humans. These alkaloids are commonly detected as contaminants in various food products, including tea, grains, milk, honey, as well as plant-derived pharmaceuticals and dietary supplements. Currently, most studies on the quantitative methods for PAs focus on a limited number of PAs and employ an additive quantification strategy, largely due to the challenges associated with chromatographic separation of isomers. These approaches limit the ability to assess exposure and health risk accurately. Herein, a method was established to quantify 35 PAs individually in dried tea samples using ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS) . The 35 target compounds were divided into two groups. The first group included 30 PAs, while the second group consisted of 5 PAs. These compounds were separated on Waters Acquity BEH C18 (150 mm×2.1 mm, 1.7 μm) and Thermo AcclaimTM C30 (150 mm×2.1 mm, 3.0 μm) chromatographic columns, respectively. Mobile phases were H2O containning 5 mmol/L ammonium formate and 0.13% formic acid (pH=3) and methanol-acetonitrile (4∶6, volume raio) containing 0.1% formic acid. The 33 target compounds were separated and 2 isomers co-eluted. Under positive-ion electrospray ionization (ESI) and multiple reaction monitoring (MRM) mode, target compounds were quantified using the external standard method with the matrix-matched standard curve. The results demonstrated that all target compounds showed good linearity (r2>0.99) in their respective mass concentration ranges. The limits of detection (LODs) and quantification (LOQs) of the method were in the range of 0.2-8.0 µg/kg and 0.5-25.0 µg/kg, respectively. The average recoveries of more than 89% compounds were in the range of 70%-130% at spiked levels of 1, 2, and 5 fold-LOQs and the relative standard deviations (RSDs) were less than 20% (RSDs of lasiocarpine and echimidine were less than 30%). Moreover, the quantitative method of the 35 PAs was applied to 21 dark tea and 30 black tea samples from Yunnan and Fujian Province, where PAs were detected in 4 dark samples with total contents ranging from 5.07 to 15.48 µg/kg and were not detected in black tea samples. The detection rate of PAs in dark tea samples was higher than that of black tea samples. That might be because most dark tea was processed from fresh leaves picked by machines, and this attribution could be associated with the mixing of weeds containing PAs during tea harvesting. And the detected concentrations of all samples were lower than the maximum levels of tea in European Union regulations, indicating that the tea samples involved in this research are basically safe. In brief, the quantitative method of the 35 PAs facilitates the analysis of the occurrence, composition and potential risks in tea samples.

pyrrolizidine alkaloids (PAs)  /  ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS)  /  tea
董璐, 张晓林, 杨晨, 赵旌妍, 王学梅, 褚莹倩, 李雪花. 超高效液相色谱-三重四极杆质谱法测定干茶中35种吡咯里西啶生物碱. 色谱, 2025 , 43 (12) : 1342 -1353 . DOI: 10.3724/SP.J.1123.2025.01020
Lu DONG, Xiaolin ZHANG, Chen YANG, Jingyan ZHAO, Xuemei WANG, Yingqian CHU, Xuehua LI. Determination of 35 pyrrolizidine alkaloids in dried tea by ultra-high performance liquid chromatography- triple quadrupole mass spectrometry[J]. Chinese Journal of Chromatography, 2025 , 43 (12) : 1342 -1353 . DOI: 10.3724/SP.J.1123.2025.01020
  • Applied Basic Research Program of Liaoning Province(2023JH2/101700338)
  • Science and Technology Program Projects of the General Administration of Customs(2024HK120)
  • Science and Technology Program Project of Dalian Customs(2023DK07)
Year 2025 volume 43 Issue 12
28
12
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Article Info
doi: 10.3724/SP.J.1123.2025.01020
  • Receive Date:2025-02-16
  • Online Date:2026-10-30
  • Published:2025-12-08
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  • Received:2025-02-16
Funding
Applied Basic Research Program of Liaoning Province(2023JH2/101700338)
Science and Technology Program Projects of the General Administration of Customs(2024HK120)
Science and Technology Program Project of Dalian Customs(2023DK07)
Affiliations
    1. Key Laboratory of Industrial Ecology and Environmental Engineering,School of Environment,Dalian University of Technology,Dalian 116024,China
    2. Technology Center of Dalian Customs District,Dalian 116001,China
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表12种不同金属材料的力学参数
科
Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)
属
Genus
种数
Number of
species
占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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