Simultaneous Determination of 21 Pyrrolizidine Alkaloids in Tea

WAN Jing-yi; FENG Chao; CHEN Yu-hang; XU Qian; LIN Yuan-jie; LE Sun-yang; LU Da-sheng; QIU Xin-lei

doi:10.19969/j.fxcsxb.23062903

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Simultaneous Determination of 21 Pyrrolizidine Alkaloids in Tea

Scientific Papers | 更新时间：2023-10-18

- Simultaneous Determination of 21 Pyrrolizidine Alkaloids in Tea
- Journal of Instrumental Analysis Vol. 42, Issue 10, Pages: 1351-1356(2023)
- 作者机构：
  
  上海市疾病预防控制中心，上海 200336
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23062903
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万静宜,冯超,陈宇航等.茶叶中21种吡咯里西啶生物碱检测方法研究[J].分析测试学报,2023,42(10):1351-1356.

WAN Jing-yi,FENG Chao,CHEN Yu-hang,et al.Simultaneous Determination of 21 Pyrrolizidine Alkaloids in Tea[J].Journal of Instrumental Analysis,2023,42(10):1351-1356.
万静宜,冯超,陈宇航等.茶叶中21种吡咯里西啶生物碱检测方法研究[J].分析测试学报,2023,42(10):1351-1356. DOI： 10.19969/j.fxcsxb.23062903.

WAN Jing-yi,FENG Chao,CHEN Yu-hang,et al.Simultaneous Determination of 21 Pyrrolizidine Alkaloids in Tea[J].Journal of Instrumental Analysis,2023,42(10):1351-1356. DOI： 10.19969/j.fxcsxb.23062903.

摘要

基于高效液相色谱-串联质谱建立了同时检测茶叶中21种吡咯里西啶生物碱（PAs）的分析方法。样品经0.05 mol/L 硫酸提取，固相萃取法净化，Phenomenex Kinetex F5 色谱柱（150 mm×3.0 mm×2.6 μm）分离，以甲醇-0.1%甲酸水作为流动相进行梯度洗脱，正离子模式扫描，多反应监测（MRM）模式下进行检测，基质匹配标准曲线外标法定量。结果表明，21种PAs在各自质量浓度范围内呈良好线性关系（,r,2,≥0.995 0），方法检出限（LOD）为0.3~1.0 μg/kg；在低、中、高3个加标水平下，回收率为72.1%~108%，相对标准偏差（RSD，,n,=6）为2.0%~9.8%。将该方法用于市售茶叶样品的检测，有5件样品检出PAs，总含量在1.8~85 μg/kg之间。所建立的方法高效、稳定，可同时实现21种吡咯里西啶生物碱的检测。

Abstract

An analytical method for the simultaneous detection of 21 pyrrolizidine alkaloids（PAs） in tea was established by high performance liquid chromatography-tandem mass spectrometry. The samples were extracted by 0.05 mol/L sulfuric acid，cleaned by solid phase extraction，separated by Phenomenex Kinetex F5 column（150 mm×3.0 mm×2.6 μm），and gradient eluted with methanol-0.1% formic acid water as mobile phase. The analytes were detected in multiple reaction monitoring（MRM） mode with positive ion mode scanning，quantified by matrix matching standard curve external standard method. The results showed that 21 PAs showed a good linear relationship in their respective concentration ranges（,r,2,≥0.995 0）. The detection limits（LODs） of the method was 0.3-1.0 μg/kg. Under the three spiked levels of low，medium and high，the recoveries（,n,=6） were between 72.1%-108%，and the relative standard deviations（RSDs，,n,=6） were 2.0%-9.8%. This method was used for the detection of commercially available tea samples，and PAs were detected in 5 samples with total content of 1.8-85 μg/kg. The established method is efficient and stable，and can simultaneously detect 21 pyrrolizidine alkaloids.

关键词

吡咯里西啶生物碱茶叶高效液相色谱-串联质谱法

Keywords

pyrrolizidine alkaloidsteahigh performance liquid chromatography-tandem mass spectrometry

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College of Chemical Engineering，Zhejiang University of Technology

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