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Quick and Green Microextraction of Pyrrolizidine Alkaloids from Infusions of Mallow, Calendula, and Hibiscus Flowers Using Ultrahigh-Performance Liquid Chromatography Coupled to Tandem Mass Spectrometry Analysis
Journal of Agricultural and Food Chemistry ( IF 5.7 ) Pub Date : 2022-06-17 , DOI: 10.1021/acs.jafc.2c02186
Natalia Casado 1 , Begoña Fernández-Pintor 1 , Sonia Morante-Zarcero 1 , Isabel Sierra 1
Affiliation  

A sustainable microextraction of pyrrolizidine alkaloids (PAs) from edible flower infusions using the innovative μSPEed technique is proposed. Different sorbents and extraction conditions were tested, achieving the highest extraction efficiency with an octadecylsilane sorbent (4 mg). The extraction procedure just took 1 min per sample, and only 300 μL of methanol and 300 μL of the sample were used per extraction. Ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry was used for analysis. The method was properly validated, providing suitable linearity, selectivity, sensitivity (quantification limits 0.3–1 μg/L), overall recoveries (79–97%), and precision (≤17% relative standard deviation). Its application to the analysis of different infusions of mallow, calendula, and hibiscus flowers revealed similar total PA values (23–41 μg/L) and contamination profile among the mallow and hibiscus samples, with predominance of senecionine-type and heliotrine-type PAs, respectively. Conversely, calendula samples showed more variations (23–113 μg/L), highlighting the occurrence of intermedine N-oxide and europine N-oxide on them.

中文翻译:

使用超高效液相色谱联用串联质谱分析法从锦葵、金盏花和芙蓉花浸液中快速、绿色地微萃取吡咯里西啶生物碱

提出了使用创新的 μSPEed 技术从可食用花浸液中可持续微萃取吡咯里西啶生物碱 (PA) 的方法。测试了不同的吸附剂和萃取条件,使用十八烷基硅烷吸附剂 (4 mg) 实现了最高萃取效率。每个样品的提取过程只需 1 分钟,每次提取仅使用 300 μL 甲醇和 300 μL 样品。使用与串联质谱联用的超高效液相色谱法进行分析。该方法经过适当验证,可提供合适的线性、选择性、灵敏度(定量限为 0.3–1 μg/L)、总回收率 (79–97%) 和精密度(≤17% 相对标准偏差)。其在锦葵、金盏花等不同浸剂分析中的应用,和芙蓉花在锦葵和芙蓉样品中显示出相似的总 PA 值 (23–41 μg/L) 和污染概况,分别以 senecionine 型和 heliotrine 型 PA 为主。相反,金盏花样品显示出更多变异 (23–113 μg/L),突显了中间体的发生N-氧化物和欧洲的N-氧化物在他们身上。
更新日期:2022-06-17
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